# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _publ_contact_author_name 'Philip C. Andrews' _publ_contact_author_address ;School of Chemistry Monash University PO Box 23 Melbourne Vic. 3800 Australia ; _publ_contact_author_email phil.andrews@sci.monash.edu.au _publ_contact_author_phone '+61 3 9905 5509' _publ_contact_author_fax '+61 3 9905 4597' loop_ _publ_author_name _publ_author_address P.C.Andrews ;School of Chemistry Monash University PO Box 23 Melbourne Vic. 3800 Australia ; M.Koutsaplis ;School of Chemistry Monash University PO Box 23 Melbourne Vic. 3800 Australia ; S.D.Bull ;Department of Chemistry University of Bath Bath BA2 7AY UK ; data_cmp1 _database_code_depnum_ccdc_archive 'CCDC 764914' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H62 Li4 N4 O7 Si' _chemical_formula_sum 'C34 H62 Li4 N4 O7 Si' _chemical_formula_weight 694.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2332(2) _cell_length_b 11.2688(2) _cell_length_c 17.5740(4) _cell_angle_alpha 88.1390(10) _cell_angle_beta 89.7480(10) _cell_angle_gamma 77.4630(10) _cell_volume 1977.19(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37027 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 30.15 _reflns_number_total 11494 _reflns_number_gt 8310 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11494 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.13877(5) 0.76133(4) 0.25257(3) 0.02316(11) Uani 1 1 d . . . O1 O 0.39317(13) 1.02853(10) 0.30528(7) 0.0281(3) Uani 1 1 d . . . O2 O 0.42746(13) 0.75943(11) 0.09524(7) 0.0285(3) Uani 1 1 d . . . O3 O 0.30606(12) 0.53514(10) 0.20599(7) 0.0264(3) Uani 1 1 d . . . O4 O 0.48741(12) 0.57607(10) 0.34645(6) 0.0232(2) Uani 1 1 d . . . O5 O 0.22623(14) 1.02303(12) 0.12202(8) 0.0350(3) Uani 1 1 d . . . O6 O 0.27071(13) 0.85900(10) 0.43959(7) 0.0284(3) Uani 1 1 d . . . O7 O 0.28130(12) 0.79742(10) 0.25440(6) 0.0216(2) Uani 1 1 d . . . N1 N 0.52012(15) 0.94698(12) 0.20781(8) 0.0246(3) Uani 1 1 d . . . N2 N 0.57171(15) 0.64988(12) 0.18109(8) 0.0244(3) Uani 1 1 d . . . N3 N 0.14931(14) 0.61218(12) 0.29178(8) 0.0235(3) Uani 1 1 d . . . N4 N 0.55286(14) 0.75250(12) 0.35856(8) 0.0221(3) Uani 1 1 d . . . C1 C 0.60730(19) 0.96635(16) 0.14429(10) 0.0289(4) Uani 1 1 d . . . H1A H 0.5528 1.0189 0.1046 0.035 Uiso 1 1 calc R . . H1B H 0.6457 0.8871 0.1216 0.035 Uiso 1 1 calc R . . C2 C 0.7207(2) 1.02483(19) 0.16794(12) 0.0373(4) Uani 1 1 d . . . H2A H 0.7778 1.0336 0.1234 0.045 Uiso 1 1 calc R . . H2B H 0.7769 0.9724 0.2070 0.045 Uiso 1 1 calc R . . C3 C 0.6636(2) 1.14917(19) 0.19989(13) 0.0414(5) Uani 1 1 d . . . H3A H 0.7340 1.1766 0.2286 0.050 Uiso 1 1 calc R . . H3B H 0.6335 1.2088 0.1576 0.050 Uiso 1 1 calc R . . C4 C 0.5476(2) 1.14323(16) 0.25151(11) 0.0342(4) Uani 1 1 d . . . H4 H 0.5127 1.2092 0.2833 0.041 Uiso 1 1 calc R . . C5 C 0.49268(18) 1.04395(14) 0.25278(9) 0.0241(3) Uani 1 1 d . . . C6 C 0.3536(3) 1.12149(17) 0.35908(12) 0.0446(6) Uani 1 1 d . . . H6A H 0.4294 1.1237 0.3925 0.067 Uiso 1 1 calc R . . H6B H 0.2792 1.1043 0.3896 0.067 Uiso 1 1 calc R . . H6C H 0.3252 1.2003 0.3321 0.067 Uiso 1 1 calc R . . C7 C 0.6799(2) 0.54255(18) 0.19439(11) 0.0347(4) Uani 1 1 d . . . H7A H 0.6440 0.4686 0.1882 0.042 Uiso 1 1 calc R . . H7B H 0.7116 0.5418 0.2476 0.042 Uiso 1 1 calc R . . C8 C 0.7971(2) 0.5380(2) 0.14147(13) 0.0432(5) Uani 1 1 d . . . H8A H 0.8683 0.4657 0.1545 0.052 Uiso 1 1 calc R . . H8B H 0.8341 0.6114 0.1471 0.052 Uiso 1 1 calc R . . C9 C 0.7513(2) 0.53181(19) 0.05959(12) 0.0407(5) Uani 1 1 d . . . H9A H 0.8192 0.5523 0.0242 0.049 Uiso 1 1 calc R . . H9B H 0.7417 0.4481 0.0496 0.049 Uiso 1 1 calc R . . C10 C 0.6192(2) 0.61969(18) 0.04615(11) 0.0348(4) Uani 1 1 d . . . H10 H 0.5866 0.6387 -0.0043 0.042 Uiso 1 1 calc R . . C11 C 0.54706(18) 0.67137(15) 0.10547(10) 0.0253(3) Uani 1 1 d . . . C12 C 0.3761(2) 0.7811(2) 0.01967(11) 0.0400(5) Uani 1 1 d . . . H12A H 0.4387 0.8155 -0.0121 0.060 Uiso 1 1 calc R . . H12B H 0.2892 0.8385 0.0204 0.060 Uiso 1 1 calc R . . H12C H 0.3652 0.7043 -0.0013 0.060 Uiso 1 1 calc R . . C13 C 0.07300(18) 0.58058(15) 0.35728(10) 0.0271(4) Uani 1 1 d . . . H13A H 0.0246 0.6558 0.3812 0.032 Uiso 1 1 calc R . . H13B H 0.1352 0.5326 0.3956 0.032 Uiso 1 1 calc R . . C14 C -0.0267(2) 0.50708(18) 0.33253(12) 0.0350(4) Uani 1 1 d . . . H14A H -0.0867 0.5534 0.2927 0.042 Uiso 1 1 calc R . . H14B H -0.0823 0.4916 0.3765 0.042 Uiso 1 1 calc R . . C15 C 0.0485(2) 0.38630(17) 0.30140(12) 0.0363(4) Uani 1 1 d . . . H15A H 0.0808 0.3283 0.3443 0.044 Uiso 1 1 calc R . . H15B H -0.0131 0.3512 0.2701 0.044 Uiso 1 1 calc R . . C16 C 0.16556(19) 0.40424(16) 0.25367(11) 0.0299(4) Uani 1 1 d . . . H16 H 0.2138 0.3385 0.2254 0.036 Uiso 1 1 calc R . . C17 C 0.20290(17) 0.51065(15) 0.25035(9) 0.0240(3) Uani 1 1 d . . . C18 C 0.3507(2) 0.45647(17) 0.14452(11) 0.0330(4) Uani 1 1 d . . . H18A H 0.3964 0.3763 0.1649 0.049 Uiso 1 1 calc R . . H18B H 0.4129 0.4910 0.1126 0.049 Uiso 1 1 calc R . . H18C H 0.2736 0.4482 0.1139 0.049 Uiso 1 1 calc R . . C19 C 0.61639(18) 0.82564(14) 0.40819(10) 0.0259(3) Uani 1 1 d . . . H19A H 0.5582 0.8494 0.4528 0.031 Uiso 1 1 calc R . . H19B H 0.6256 0.9010 0.3801 0.031 Uiso 1 1 calc R . . C20 C 0.75355(18) 0.75719(15) 0.43564(11) 0.0290(4) Uani 1 1 d . . . H20A H 0.7958 0.8114 0.4659 0.035 Uiso 1 1 calc R . . H20B H 0.8116 0.7312 0.3913 0.035 Uiso 1 1 calc R . . C21 C 0.74006(19) 0.64607(16) 0.48433(10) 0.0286(4) Uani 1 1 d . . . H21A H 0.8286 0.5900 0.4904 0.034 Uiso 1 1 calc R . . H21B H 0.7066 0.6716 0.5355 0.034 Uiso 1 1 calc R . . C22 C 0.64425(18) 0.58232(15) 0.44665(10) 0.0257(3) Uani 1 1 d . . . H22 H 0.6373 0.5034 0.4644 0.031 Uiso 1 1 calc R . . C23 C 0.56820(16) 0.63693(14) 0.38767(9) 0.0211(3) Uani 1 1 d . . . C24 C 0.5035(2) 0.44827(15) 0.36060(11) 0.0300(4) Uani 1 1 d . . . H24A H 0.5970 0.4077 0.3519 0.045 Uiso 1 1 calc R . . H24B H 0.4453 0.4164 0.3262 0.045 Uiso 1 1 calc R . . H24C H 0.4793 0.4329 0.4135 0.045 Uiso 1 1 calc R . . C25 C 0.2717(2) 1.1044(2) 0.06945(15) 0.0501(6) Uani 1 1 d . . . H25A H 0.3297 1.0590 0.0301 0.060 Uiso 1 1 calc R . . H25B H 0.3224 1.1562 0.0960 0.060 Uiso 1 1 calc R . . C26 C 0.1461(3) 1.1797(3) 0.03462(18) 0.0741(9) Uani 1 1 d . . . H26A H 0.1593 1.2607 0.0172 0.089 Uiso 1 1 calc R . . H26B H 0.1165 1.1386 -0.0090 0.089 Uiso 1 1 calc R . . C27 C 0.0485(3) 1.1902(3) 0.09759(19) 0.0754(9) Uani 1 1 d . . . H27A H -0.0383 1.1768 0.0792 0.091 Uiso 1 1 calc R . . H27B H 0.0338 1.2719 0.1194 0.091 Uiso 1 1 calc R . . C28 C 0.1083(3) 1.0940(2) 0.15617(15) 0.0533(6) Uani 1 1 d . . . H28A H 0.1317 1.1315 0.2029 0.064 Uiso 1 1 calc R . . H28B H 0.0442 1.0423 0.1697 0.064 Uiso 1 1 calc R . . C29 C 0.2261(3) 0.94183(19) 0.49912(12) 0.0439(5) Uani 1 1 d . . . H29A H 0.1467 1.0041 0.4823 0.053 Uiso 1 1 calc R . . H29B H 0.2978 0.9835 0.5134 0.053 Uiso 1 1 calc R . . C30 C 0.1906(3) 0.8665(2) 0.56660(12) 0.0477(6) Uani 1 1 d . . . H30A H 0.2647 0.8474 0.6041 0.057 Uiso 1 1 calc R . . H30B H 0.1084 0.9097 0.5922 0.057 Uiso 1 1 calc R . . C31 C 0.1688(2) 0.75303(19) 0.53054(12) 0.0387(5) Uani 1 1 d . . . H31A H 0.0778 0.7650 0.5085 0.046 Uiso 1 1 calc R . . H31B H 0.1838 0.6830 0.5673 0.046 Uiso 1 1 calc R . . C32 C 0.2752(2) 0.73702(16) 0.46929(11) 0.0323(4) Uani 1 1 d . . . H32A H 0.3645 0.7004 0.4910 0.039 Uiso 1 1 calc R . . H32B H 0.2548 0.6845 0.4289 0.039 Uiso 1 1 calc R . . C33 C 0.01456(19) 0.86530(16) 0.31166(11) 0.0316(4) Uani 1 1 d . . . H33A H 0.0445 0.8576 0.3648 0.047 Uiso 1 1 calc R . . H33B H -0.0728 0.8434 0.3082 0.047 Uiso 1 1 calc R . . H33C H 0.0067 0.9494 0.2930 0.047 Uiso 1 1 calc R . . C34 C 0.0723(2) 0.76425(17) 0.15359(11) 0.0325(4) Uani 1 1 d . . . H34A H 0.0744 0.8426 0.1282 0.049 Uiso 1 1 calc R . . H34B H -0.0201 0.7533 0.1554 0.049 Uiso 1 1 calc R . . H34C H 0.1277 0.6984 0.1252 0.049 Uiso 1 1 calc R . . Li1 Li 0.5886(3) 0.7812(3) 0.24967(16) 0.0259(6) Uani 1 1 d . . . Li2 Li 0.4126(3) 0.6471(2) 0.24761(16) 0.0249(6) Uani 1 1 d . . . Li3 Li 0.3551(3) 0.8845(3) 0.17515(17) 0.0292(6) Uani 1 1 d . . . Li4 Li 0.3644(3) 0.8586(3) 0.33720(16) 0.0257(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0239(2) 0.0237(2) 0.0218(2) 0.00138(16) -0.00047(18) -0.00511(17) O1 0.0382(7) 0.0215(5) 0.0236(6) -0.0020(4) 0.0055(5) -0.0044(5) O2 0.0355(7) 0.0325(6) 0.0181(6) -0.0006(5) -0.0014(5) -0.0083(5) O3 0.0306(7) 0.0266(6) 0.0247(6) -0.0069(5) 0.0056(5) -0.0113(5) O4 0.0305(6) 0.0192(5) 0.0211(6) 0.0005(4) -0.0035(5) -0.0082(5) O5 0.0361(8) 0.0322(7) 0.0344(7) 0.0100(5) 0.0016(6) -0.0044(6) O6 0.0393(7) 0.0231(6) 0.0229(6) -0.0021(5) 0.0046(5) -0.0068(5) O7 0.0248(6) 0.0227(5) 0.0183(5) 0.0004(4) 0.0000(4) -0.0072(4) N1 0.0309(8) 0.0228(6) 0.0220(7) 0.0000(5) 0.0024(6) -0.0097(6) N2 0.0302(8) 0.0241(7) 0.0195(7) -0.0033(5) 0.0028(6) -0.0070(6) N3 0.0252(7) 0.0240(6) 0.0215(7) -0.0006(5) 0.0031(6) -0.0058(5) N4 0.0284(7) 0.0188(6) 0.0194(7) -0.0015(5) -0.0020(5) -0.0058(5) C1 0.0330(10) 0.0269(8) 0.0276(9) 0.0024(7) 0.0054(7) -0.0089(7) C2 0.0292(10) 0.0428(11) 0.0419(12) 0.0088(9) 0.0003(8) -0.0135(8) C3 0.0504(13) 0.0391(10) 0.0425(12) 0.0019(9) -0.0035(10) -0.0268(10) C4 0.0486(12) 0.0249(8) 0.0323(10) -0.0019(7) -0.0011(9) -0.0149(8) C5 0.0293(9) 0.0214(7) 0.0213(8) 0.0032(6) -0.0025(7) -0.0049(6) C6 0.0744(16) 0.0224(9) 0.0331(11) -0.0051(7) 0.0170(10) -0.0016(9) C7 0.0354(11) 0.0352(9) 0.0315(10) -0.0029(8) 0.0019(8) -0.0030(8) C8 0.0388(12) 0.0430(11) 0.0466(13) -0.0085(9) 0.0071(10) -0.0054(9) C9 0.0474(13) 0.0396(10) 0.0343(11) -0.0122(8) 0.0156(9) -0.0059(9) C10 0.0446(12) 0.0397(10) 0.0220(9) -0.0072(7) 0.0060(8) -0.0129(9) C11 0.0322(9) 0.0254(8) 0.0208(8) -0.0035(6) 0.0022(7) -0.0115(7) C12 0.0516(13) 0.0481(11) 0.0207(9) 0.0041(8) -0.0074(9) -0.0123(10) C13 0.0285(9) 0.0271(8) 0.0254(9) 0.0009(6) 0.0041(7) -0.0057(7) C14 0.0299(10) 0.0379(10) 0.0397(11) -0.0020(8) 0.0078(8) -0.0131(8) C15 0.0376(11) 0.0315(9) 0.0434(12) -0.0020(8) 0.0084(9) -0.0153(8) C16 0.0326(10) 0.0264(8) 0.0321(10) -0.0036(7) 0.0062(8) -0.0092(7) C17 0.0253(8) 0.0259(8) 0.0211(8) -0.0010(6) -0.0011(6) -0.0063(6) C18 0.0399(11) 0.0346(9) 0.0280(9) -0.0114(7) 0.0094(8) -0.0147(8) C19 0.0308(9) 0.0211(7) 0.0257(9) -0.0031(6) -0.0030(7) -0.0051(6) C20 0.0265(9) 0.0269(8) 0.0341(10) -0.0038(7) -0.0044(7) -0.0066(7) C21 0.0294(9) 0.0296(8) 0.0254(9) 0.0000(7) -0.0050(7) -0.0034(7) C22 0.0307(9) 0.0231(7) 0.0234(8) 0.0010(6) -0.0029(7) -0.0060(6) C23 0.0245(8) 0.0220(7) 0.0169(7) -0.0034(5) 0.0022(6) -0.0052(6) C24 0.0409(11) 0.0206(8) 0.0302(9) 0.0026(6) -0.0070(8) -0.0107(7) C25 0.0477(14) 0.0473(12) 0.0549(15) 0.0191(11) 0.0025(11) -0.0123(10) C26 0.0631(18) 0.0764(19) 0.075(2) 0.0463(16) -0.0116(15) -0.0057(15) C27 0.0639(19) 0.0611(17) 0.083(2) 0.0251(15) 0.0108(16) 0.0214(14) C28 0.0622(16) 0.0394(12) 0.0527(15) 0.0046(10) 0.0149(12) 0.0003(11) C29 0.0612(15) 0.0340(10) 0.0373(12) -0.0115(8) 0.0090(10) -0.0109(10) C30 0.0644(16) 0.0470(12) 0.0302(11) -0.0082(9) 0.0134(10) -0.0084(11) C31 0.0387(11) 0.0395(10) 0.0364(11) 0.0040(8) 0.0100(9) -0.0056(8) C32 0.0380(11) 0.0257(8) 0.0321(10) 0.0013(7) 0.0056(8) -0.0053(7) C33 0.0303(10) 0.0282(8) 0.0339(10) 0.0037(7) 0.0016(8) -0.0017(7) C34 0.0326(10) 0.0358(9) 0.0307(10) 0.0051(7) -0.0061(8) -0.0118(8) Li1 0.0331(16) 0.0236(13) 0.0216(14) -0.0012(10) 0.0009(12) -0.0077(11) Li2 0.0303(16) 0.0227(13) 0.0229(14) -0.0022(10) 0.0011(12) -0.0079(11) Li3 0.0348(17) 0.0294(14) 0.0246(15) 0.0034(11) 0.0002(13) -0.0104(12) Li4 0.0322(16) 0.0229(13) 0.0221(14) -0.0010(10) -0.0017(12) -0.0059(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O7 1.5977(12) . ? Si1 N3 1.7772(14) . ? Si1 C34 1.8673(19) . ? Si1 C33 1.8676(19) . ? Si1 Li2 2.820(3) . ? Si1 Li3 3.141(3) . ? Si1 Li4 3.160(3) . ? O1 C5 1.406(2) . ? O1 C6 1.426(2) . ? O1 Li4 2.059(3) . ? O2 C11 1.406(2) . ? O2 C12 1.424(2) . ? O2 Li3 2.043(3) . ? O3 C17 1.380(2) . ? O3 C18 1.430(2) . ? O3 Li2 1.995(3) . ? O4 C23 1.4009(19) . ? O4 C24 1.4273(18) . ? O4 Li2 1.975(3) . ? O5 C25 1.428(2) . ? O5 C28 1.436(3) . ? O5 Li3 2.017(3) . ? O6 C29 1.431(2) . ? O6 C32 1.446(2) . ? O6 Li4 2.035(3) . ? O7 Li4 1.910(3) . ? O7 Li3 1.923(3) . ? O7 Li2 1.927(3) . ? N1 C5 1.348(2) . ? N1 C1 1.466(2) . ? N1 Li1 1.967(3) . ? N1 Li3 2.056(3) . ? N2 C11 1.358(2) . ? N2 C7 1.465(2) . ? N2 Li1 1.975(3) . ? N2 Li2 2.006(3) . ? N3 C17 1.385(2) . ? N3 C13 1.466(2) . ? N4 C23 1.3605(19) . ? N4 C19 1.465(2) . ? N4 Li1 1.976(3) . ? N4 Li4 2.065(3) . ? C1 C2 1.519(3) . ? C1 Li1 2.782(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.521(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.502(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.357(2) . ? C4 H4 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.507(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.523(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.507(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.348(3) . ? C10 H10 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.520(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.528(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.505(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.335(2) . ? C16 H16 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.520(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.524(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.503(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.348(2) . ? C22 H22 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.498(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.478(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.502(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.524(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.505(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.515(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? Li1 Li2 2.591(4) . ? Li1 Li3 2.739(4) . ? Li1 Li4 2.752(4) . ? Li2 Li4 2.851(4) . ? Li2 Li3 2.868(4) . ? Li3 Li4 2.853(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Si1 N3 110.94(7) . . ? O7 Si1 C34 112.03(8) . . ? N3 Si1 C34 107.28(8) . . ? O7 Si1 C33 110.89(8) . . ? N3 Si1 C33 106.33(8) . . ? C34 Si1 C33 109.14(9) . . ? O7 Si1 Li2 41.06(7) . . ? N3 Si1 Li2 74.52(7) . . ? C34 Si1 Li2 106.96(9) . . ? C33 Si1 Li2 141.56(9) . . ? O7 Si1 Li3 29.68(7) . . ? N3 Si1 Li3 131.46(8) . . ? C34 Si1 Li3 83.90(8) . . ? C33 Si1 Li3 114.24(8) . . ? Li2 Si1 Li3 57.22(8) . . ? O7 Si1 Li4 28.32(7) . . ? N3 Si1 Li4 104.80(7) . . ? C34 Si1 Li4 137.51(8) . . ? C33 Si1 Li4 87.34(8) . . ? Li2 Si1 Li4 56.61(8) . . ? Li3 Si1 Li4 53.86(8) . . ? C5 O1 C6 116.88(14) . . ? C5 O1 Li4 121.66(13) . . ? C6 O1 Li4 116.23(14) . . ? C11 O2 C12 117.01(14) . . ? C11 O2 Li3 122.61(13) . . ? C12 O2 Li3 118.31(14) . . ? C17 O3 C18 117.49(13) . . ? C17 O3 Li2 117.18(13) . . ? C18 O3 Li2 123.26(14) . . ? C23 O4 C24 117.79(12) . . ? C23 O4 Li2 119.00(12) . . ? C24 O4 Li2 118.79(13) . . ? C25 O5 C28 105.35(16) . . ? C25 O5 Li3 121.49(16) . . ? C28 O5 Li3 124.69(15) . . ? C29 O6 C32 108.15(14) . . ? C29 O6 Li4 138.34(14) . . ? C32 O6 Li4 111.81(13) . . ? Si1 O7 Li4 128.30(12) . . ? Si1 O7 Li3 126.03(11) . . ? Li4 O7 Li3 96.22(14) . . ? Si1 O7 Li2 105.94(10) . . ? Li4 O7 Li2 96.00(13) . . ? Li3 O7 Li2 96.33(14) . . ? C5 N1 C1 111.53(13) . . ? C5 N1 Li1 121.78(14) . . ? C1 N1 Li1 107.35(14) . . ? C5 N1 Li3 114.51(15) . . ? C1 N1 Li3 113.62(14) . . ? Li1 N1 Li3 85.77(13) . . ? C11 N2 C7 110.94(14) . . ? C11 N2 Li1 121.86(14) . . ? C7 N2 Li1 110.99(14) . . ? C11 N2 Li2 116.51(14) . . ? C7 N2 Li2 112.29(14) . . ? Li1 N2 Li2 81.22(13) . . ? C17 N3 C13 111.28(13) . . ? C17 N3 Si1 121.03(11) . . ? C13 N3 Si1 125.48(11) . . ? C23 N4 C19 110.62(13) . . ? C23 N4 Li1 120.11(13) . . ? C19 N4 Li1 112.33(14) . . ? C23 N4 Li4 120.72(14) . . ? C19 N4 Li4 104.47(13) . . ? Li1 N4 Li4 85.83(13) . . ? N1 C1 C2 113.07(16) . . ? N1 C1 Li1 42.45(10) . . ? C2 C1 Li1 108.78(13) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? Li1 C1 H1A 140.1 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? Li1 C1 H1B 71.2 . . ? H1A C1 H1B 107.8 . . ? C1 C2 C3 109.75(17) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 110.27(15) . . ? C4 C3 H3A 109.6 . . ? C2 C3 H3A 109.6 . . ? C4 C3 H3B 109.6 . . ? C2 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 120.16(18) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C5 C4 128.63(17) . . ? N1 C5 O1 109.02(13) . . ? C4 C5 O1 122.35(16) . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 113.42(16) . . ? N2 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N2 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C9 109.49(18) . . ? C7 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? C7 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 110.04(16) . . ? C10 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 120.22(18) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 N2 128.63(17) . . ? C10 C11 O2 122.02(16) . . ? N2 C11 O2 109.34(14) . . ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 110.51(15) . . ? N3 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 109.59(16) . . ? C13 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? C13 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C14 110.71(15) . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C15 121.28(17) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 O3 124.57(16) . . ? C16 C17 N3 126.50(16) . . ? O3 C17 N3 108.89(13) . . ? O3 C18 H18A 109.5 . . ? O3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 C20 112.09(13) . . ? N4 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N4 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C19 C20 C21 109.95(15) . . ? C19 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 . . ? C19 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C22 C21 C20 109.38(14) . . ? C22 C21 H21A 109.8 . . ? C20 C21 H21A 109.8 . . ? C22 C21 H21B 109.8 . . ? C20 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C23 C22 C21 120.08(15) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 N4 129.29(15) . . ? C22 C23 O4 121.71(14) . . ? N4 C23 O4 108.99(13) . . ? O4 C24 H24A 109.5 . . ? O4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O5 C25 C26 104.49(19) . . ? O5 C25 H25A 110.9 . . ? C26 C25 H25A 110.9 . . ? O5 C25 H25B 110.9 . . ? C26 C25 H25B 110.9 . . ? H25A C25 H25B 108.9 . . ? C27 C26 C25 103.4(2) . . ? C27 C26 H26A 111.1 . . ? C25 C26 H26A 111.1 . . ? C27 C26 H26B 111.1 . . ? C25 C26 H26B 111.1 . . ? H26A C26 H26B 109.0 . . ? C26 C27 C28 106.1(2) . . ? C26 C27 H27A 110.5 . . ? C28 C27 H27A 110.5 . . ? C26 C27 H27B 110.5 . . ? C28 C27 H27B 110.5 . . ? H27A C27 H27B 108.7 . . ? O5 C28 C27 106.0(2) . . ? O5 C28 H28A 110.5 . . ? C27 C28 H28A 110.5 . . ? O5 C28 H28B 110.5 . . ? C27 C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? O6 C29 C30 106.72(16) . . ? O6 C29 H29A 110.4 . . ? C30 C29 H29A 110.4 . . ? O6 C29 H29B 110.4 . . ? C30 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C31 C30 C29 103.24(17) . . ? C31 C30 H30A 111.1 . . ? C29 C30 H30A 111.1 . . ? C31 C30 H30B 111.1 . . ? C29 C30 H30B 111.1 . . ? H30A C30 H30B 109.1 . . ? C30 C31 C32 100.68(17) . . ? C30 C31 H31A 111.6 . . ? C32 C31 H31A 111.6 . . ? C30 C31 H31B 111.6 . . ? C32 C31 H31B 111.6 . . ? H31A C31 H31B 109.4 . . ? O6 C32 C31 104.36(15) . . ? O6 C32 H32A 110.9 . . ? C31 C32 H32A 110.9 . . ? O6 C32 H32B 110.9 . . ? C31 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N1 Li1 N2 114.89(15) . . ? N1 Li1 N4 116.51(16) . . ? N2 Li1 N4 116.06(15) . . ? N1 Li1 Li2 113.04(15) . . ? N2 Li1 Li2 49.91(10) . . ? N4 Li1 Li2 76.27(12) . . ? N1 Li1 Li3 48.48(10) . . ? N2 Li1 Li3 79.09(12) . . ? N4 Li1 Li3 110.17(15) . . ? Li2 Li1 Li3 65.05(11) . . ? N1 Li1 Li4 78.08(12) . . ? N2 Li1 Li4 113.21(15) . . ? N4 Li1 Li4 48.44(10) . . ? Li2 Li1 Li4 64.41(11) . . ? Li3 Li1 Li4 62.61(11) . . ? N1 Li1 C1 30.20(7) . . ? N2 Li1 C1 100.70(12) . . ? N4 Li1 C1 141.68(14) . . ? Li2 Li1 C1 125.69(13) . . ? Li3 Li1 C1 64.97(10) . . ? Li4 Li1 C1 108.25(12) . . ? O7 Li2 O4 114.54(15) . . ? O7 Li2 O3 102.54(15) . . ? O4 Li2 O3 107.40(13) . . ? O7 Li2 N2 116.78(15) . . ? O4 Li2 N2 105.31(15) . . ? O3 Li2 N2 109.95(15) . . ? O7 Li2 Li1 85.71(12) . . ? O4 Li2 Li1 86.99(13) . . ? O3 Li2 Li1 157.94(16) . . ? N2 Li2 Li1 48.88(10) . . ? O7 Li2 Si1 33.00(6) . . ? O4 Li2 Si1 114.11(13) . . ? O3 Li2 Si1 71.30(10) . . ? N2 Li2 Si1 138.28(14) . . ? Li1 Li2 Si1 118.70(12) . . ? O7 Li2 Li4 41.78(9) . . ? O4 Li2 Li4 79.50(11) . . ? O3 Li2 Li4 137.27(16) . . ? N2 Li2 Li4 108.40(13) . . ? Li1 Li2 Li4 60.54(11) . . ? Si1 Li2 Li4 67.71(9) . . ? O7 Li2 Li3 41.78(9) . . ? O4 Li2 Li3 136.12(14) . . ? O3 Li2 Li3 113.46(14) . . ? N2 Li2 Li3 75.43(11) . . ? Li1 Li2 Li3 59.97(11) . . ? Si1 Li2 Li3 67.02(9) . . ? Li4 Li2 Li3 59.85(10) . . ? O7 Li3 O5 116.25(17) . . ? O7 Li3 O2 105.78(14) . . ? O5 Li3 O2 107.43(15) . . ? O7 Li3 N1 114.19(15) . . ? O5 Li3 N1 108.20(14) . . ? O2 Li3 N1 104.04(15) . . ? O7 Li3 Li1 81.70(12) . . ? O5 Li3 Li1 153.96(16) . . ? O2 Li3 Li1 83.48(13) . . ? N1 Li3 Li1 45.75(9) . . ? O7 Li3 Li4 41.72(9) . . ? O5 Li3 Li4 121.27(15) . . ? O2 Li3 Li4 129.43(14) . . ? N1 Li3 Li4 74.38(12) . . ? Li1 Li3 Li4 58.93(11) . . ? O7 Li3 Li2 41.88(9) . . ? O5 Li3 Li2 150.57(16) . . ? O2 Li3 Li2 71.37(11) . . ? N1 Li3 Li2 100.35(13) . . ? Li1 Li3 Li2 54.99(10) . . ? Li4 Li3 Li2 59.78(10) . . ? O7 Li3 Si1 24.29(6) . . ? O5 Li3 Si1 96.87(12) . . ? O2 Li3 Si1 100.05(11) . . ? N1 Li3 Si1 137.64(13) . . ? Li1 Li3 Si1 104.55(11) . . ? Li4 Li3 Si1 63.41(9) . . ? Li2 Li3 Si1 55.77(8) . . ? O7 Li4 O6 115.99(16) . . ? O7 Li4 O1 108.22(14) . . ? O6 Li4 O1 111.93(14) . . ? O7 Li4 N4 110.72(15) . . ? O6 Li4 N4 103.55(13) . . ? O1 Li4 N4 105.94(14) . . ? O7 Li4 Li1 81.54(12) . . ? O6 Li4 Li1 149.26(15) . . ? O1 Li4 Li1 83.15(12) . . ? N4 Li4 Li1 45.73(9) . . ? O7 Li4 Li2 42.22(9) . . ? O6 Li4 Li2 120.53(14) . . ? O1 Li4 Li2 127.09(14) . . ? N4 Li4 Li2 69.08(11) . . ? Li1 Li4 Li2 55.05(10) . . ? O7 Li4 Li3 42.06(9) . . ? O6 Li4 Li3 150.72(16) . . ? O1 Li4 Li3 70.92(11) . . ? N4 Li4 Li3 103.40(14) . . ? Li1 Li4 Li3 58.46(11) . . ? Li2 Li4 Li3 60.37(10) . . ? O7 Li4 Si1 23.38(6) . . ? O6 Li4 Si1 92.82(11) . . ? O1 Li4 Si1 117.88(12) . . ? N4 Li4 Si1 122.77(12) . . ? Li1 Li4 Si1 103.73(11) . . ? Li2 Li4 Si1 55.68(8) . . ? Li3 Li4 Si1 62.73(8) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 30.15 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.710 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.055 data_cmp2 _database_code_depnum_ccdc_archive 'CCDC 764915' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H88 Li4 N10 O4' _chemical_formula_sum 'C42 H88 Li4 N10 O4' _chemical_formula_weight 824.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.061(2) _cell_length_b 14.802(3) _cell_length_c 17.141(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.52(3) _cell_angle_gamma 90.00 _cell_volume 2552.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19631 _diffrn_reflns_av_R_equivalents 0.1284 _diffrn_reflns_av_sigmaI/netI 0.0997 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4484 _reflns_number_gt 2494 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4484 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1393 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2035 _refine_ls_wR_factor_gt 0.1732 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.9540(2) 0.97658(13) 0.22197(10) 0.0379(6) Uani 1 1 d . . . O2 O 1.0285(2) 1.22148(14) 0.38320(11) 0.0460(6) Uani 1 1 d . B . N1 N 0.8666(2) 1.11390(15) 0.23257(12) 0.0315(6) Uani 1 1 d . B . N2 N 1.1572(2) 1.12593(15) 0.31962(12) 0.0300(6) Uani 1 1 d . B . N3 N 1.0971(3) 1.29612(17) 0.18059(15) 0.0439(7) Uani 1 1 d . B . N4 N 1.1348(3) 1.1270(2) 0.09987(14) 0.0533(8) Uani 1 1 d . B . N5 N 0.8753(2) 1.00150(17) 0.41614(12) 0.0357(6) Uani 1 1 d . . . C1 C 0.7474(3) 1.1707(2) 0.22958(18) 0.0404(8) Uani 1 1 d . . . H1A H 0.7746 1.2349 0.2335 0.049 Uiso 1 1 calc R . . H1B H 0.6916 1.1568 0.2753 0.049 Uiso 1 1 calc R . . C2 C 0.6651(3) 1.1583(2) 0.15619(18) 0.0510(9) Uani 1 1 d . . . H2A H 0.7187 1.1748 0.1102 0.061 Uiso 1 1 calc R . . H2B H 0.5867 1.1986 0.1577 0.061 Uiso 1 1 calc R . . C3 C 0.6193(3) 1.0602(3) 0.14889(19) 0.0523(9) Uani 1 1 d . . . H3A H 0.5437 1.0495 0.1843 0.063 Uiso 1 1 calc R . . H3B H 0.5887 1.0484 0.0948 0.063 Uiso 1 1 calc R . . C4 C 0.7311(3) 0.9971(2) 0.16940(17) 0.0414(8) Uani 1 1 d . . . H4 H 0.7247 0.9347 0.1569 0.050 Uiso 1 1 calc R . . C5 C 0.8406(3) 1.0294(2) 0.20555(15) 0.0316(7) Uani 1 1 d . . . C6 C 0.9571(4) 0.8873(2) 0.19132(18) 0.0513(9) Uani 1 1 d . . . H6A H 0.8896 0.8504 0.2171 0.077 Uiso 1 1 calc R . . H6B H 1.0451 0.8609 0.2006 0.077 Uiso 1 1 calc R . . H6C H 0.9386 0.8891 0.1351 0.077 Uiso 1 1 calc R . . C7 C 1.2827(3) 1.0777(2) 0.3161(2) 0.0507(9) Uani 1 1 d . . . H7A H 1.2904 1.0503 0.2637 0.061 Uiso 1 1 calc R A 1 H7B H 1.2803 1.0277 0.3545 0.061 Uiso 1 1 calc R A 1 C8A C 1.4027(4) 1.1317(4) 0.3314(3) 0.0407(17) Uani 0.797(13) 1 d P B 1 H8A H 1.4125 1.1773 0.2895 0.049 Uiso 0.797(13) 1 calc PR B 1 H8B H 1.4816 1.0918 0.3304 0.049 Uiso 0.797(13) 1 calc PR B 1 C8B C 1.3862(16) 1.0905(14) 0.3680(12) 0.033(6) Uiso 0.203(13) 1 d P B 2 H8B1 H 1.4701 1.0811 0.3394 0.040 Uiso 0.203(13) 1 calc PR B 2 H8B2 H 1.3809 1.0424 0.4080 0.040 Uiso 0.203(13) 1 calc PR B 2 C9 C 1.3968(3) 1.1794(2) 0.40985(18) 0.0472(9) Uani 1 1 d . . . H9A H 1.4181 1.1360 0.4521 0.057 Uiso 1 1 calc R B 1 H9B H 1.4634 1.2286 0.4116 0.057 Uiso 1 1 calc R B 1 C10 C 1.2601(3) 1.2180(2) 0.42207(17) 0.0412(8) Uani 1 1 d . B . H10 H 1.2452 1.2623 0.4612 0.049 Uiso 1 1 calc R . . C11 C 1.1589(3) 1.18849(19) 0.37632(16) 0.0309(7) Uani 1 1 d . . . C12 C 1.0049(4) 1.2948(3) 0.4350(2) 0.0694(12) Uani 1 1 d . . . H12A H 1.0272 1.2764 0.4885 0.104 Uiso 1 1 calc R B . H12B H 0.9109 1.3120 0.4321 0.104 Uiso 1 1 calc R . . H12C H 1.0602 1.3464 0.4202 0.104 Uiso 1 1 calc R . . C13 C 0.9933(4) 1.3618(3) 0.2010(3) 0.0817(14) Uani 1 1 d . . . H13A H 1.0208 1.4223 0.1846 0.123 Uiso 1 1 calc R . . H13B H 0.9800 1.3612 0.2576 0.123 Uiso 1 1 calc R . . H13C H 0.9100 1.3456 0.1744 0.123 Uiso 1 1 calc R . . C14 C 1.2205(3) 1.3224(2) 0.22008(19) 0.0489(9) Uani 1 1 d . . . H14A H 1.2888 1.2765 0.2107 0.073 Uiso 1 1 calc R . . H14B H 1.2050 1.3276 0.2763 0.073 Uiso 1 1 calc R . . H14C H 1.2506 1.3807 0.1997 0.073 Uiso 1 1 calc R . . C15 C 1.1141(5) 1.2937(3) 0.0974(2) 0.0751(13) Uani 1 1 d . . . H15A H 1.1599 1.3495 0.0805 0.090 Uiso 1 1 calc R . . H15B H 1.0257 1.2921 0.0716 0.090 Uiso 1 1 calc R . . C16 C 1.1931(4) 1.2133(3) 0.0724(2) 0.0795(15) Uani 1 1 d . . . H16A H 1.1978 1.2124 0.0147 0.095 Uiso 1 1 calc R . . H16B H 1.2849 1.2189 0.0931 0.095 Uiso 1 1 calc R . . C17 C 1.0126(4) 1.1077(3) 0.05516(17) 0.0572(10) Uani 1 1 d . . . H17A H 0.9487 1.1568 0.0628 0.086 Uiso 1 1 calc R . . H17B H 0.9740 1.0507 0.0733 0.086 Uiso 1 1 calc R . . H17C H 1.0337 1.1027 -0.0004 0.086 Uiso 1 1 calc R . . C18 C 1.2262(4) 1.0522(3) 0.0908(2) 0.0872(15) Uani 1 1 d . . . H18A H 1.2482 1.0452 0.0356 0.131 Uiso 1 1 calc R . . H18B H 1.1846 0.9966 0.1097 0.131 Uiso 1 1 calc R . . H18C H 1.3075 1.0641 0.1210 0.131 Uiso 1 1 calc R . . C19 C 0.8729(4) 0.9050(2) 0.39389(17) 0.0494(9) Uani 1 1 d . . . H19A H 0.9642 0.8828 0.3888 0.074 Uiso 1 1 calc R . . H19B H 0.8257 0.8980 0.3440 0.074 Uiso 1 1 calc R . . H19C H 0.8272 0.8701 0.4342 0.074 Uiso 1 1 calc R . . C20 C 0.7387(3) 1.0370(3) 0.41253(17) 0.0501(9) Uani 1 1 d . . . H20A H 0.6831 1.0041 0.4496 0.075 Uiso 1 1 calc R . . H20B H 0.7027 1.0292 0.3596 0.075 Uiso 1 1 calc R . . H20C H 0.7393 1.1014 0.4259 0.075 Uiso 1 1 calc R . . C21 C 0.9283(3) 1.0133(2) 0.49627(15) 0.0376(8) Uani 1 1 d . . . H21A H 0.8751 0.9763 0.5326 0.045 Uiso 1 1 calc R . . H21B H 0.9186 1.0774 0.5117 0.045 Uiso 1 1 calc R . . Li1 Li 1.0588(5) 1.1591(3) 0.2166(2) 0.0340(12) Uani 1 1 d . . . Li2 Li 0.9723(5) 1.0775(4) 0.3292(3) 0.0443(14) Uani 1 1 d . B . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0435(13) 0.0310(13) 0.0391(12) 0.0023(9) -0.0015(10) 0.0020(10) O2 0.0420(14) 0.0486(15) 0.0474(13) -0.0039(10) 0.0070(11) 0.0115(11) N1 0.0306(14) 0.0309(15) 0.0331(13) 0.0041(11) -0.0014(11) -0.0001(12) N2 0.0293(14) 0.0272(14) 0.0334(13) -0.0015(10) 0.0008(11) -0.0005(11) N3 0.0425(17) 0.0390(17) 0.0500(17) 0.0139(12) -0.0076(13) -0.0060(14) N4 0.0489(19) 0.073(2) 0.0382(15) -0.0090(14) 0.0096(14) -0.0098(17) N5 0.0333(15) 0.0450(17) 0.0289(13) 0.0058(11) -0.0024(11) -0.0058(13) C1 0.0354(19) 0.0335(19) 0.052(2) 0.0093(14) 0.0003(16) -0.0003(15) C2 0.037(2) 0.068(3) 0.047(2) 0.0141(17) -0.0070(16) 0.0105(19) C3 0.037(2) 0.073(3) 0.047(2) 0.0002(17) -0.0094(16) -0.0035(19) C4 0.042(2) 0.044(2) 0.0380(18) -0.0044(14) -0.0079(15) -0.0065(17) C5 0.0338(18) 0.0353(19) 0.0256(15) 0.0066(13) 0.0008(14) 0.0000(15) C6 0.069(2) 0.036(2) 0.050(2) -0.0008(15) 0.0029(18) 0.0072(18) C7 0.045(2) 0.048(2) 0.059(2) -0.0194(17) -0.0107(17) 0.0116(18) C8A 0.028(2) 0.041(3) 0.053(3) 0.008(2) 0.006(2) 0.0028(19) C9 0.047(2) 0.045(2) 0.049(2) 0.0083(16) -0.0125(16) -0.0118(17) C10 0.055(2) 0.0343(19) 0.0338(17) -0.0060(13) 0.0020(16) -0.0051(16) C11 0.0326(18) 0.0282(17) 0.0319(16) -0.0003(13) 0.0033(14) 0.0033(14) C12 0.084(3) 0.068(3) 0.057(2) -0.0085(19) 0.022(2) 0.033(2) C13 0.057(3) 0.036(2) 0.152(4) 0.027(2) -0.006(3) 0.002(2) C14 0.056(2) 0.034(2) 0.057(2) 0.0096(15) -0.0055(18) -0.0053(17) C15 0.101(4) 0.073(3) 0.050(2) 0.025(2) -0.012(2) -0.039(3) C16 0.078(3) 0.122(4) 0.039(2) -0.006(2) 0.024(2) -0.047(3) C17 0.066(3) 0.075(3) 0.0306(18) -0.0049(17) 0.0073(18) -0.016(2) C18 0.072(3) 0.117(4) 0.073(3) -0.027(3) 0.019(2) 0.021(3) C19 0.066(2) 0.046(2) 0.0352(17) 0.0027(15) -0.0069(16) -0.0162(18) C20 0.035(2) 0.075(3) 0.0400(19) 0.0122(16) -0.0040(15) -0.0047(18) C21 0.0407(18) 0.049(2) 0.0227(15) 0.0052(13) 0.0004(14) -0.0046(16) Li1 0.038(3) 0.035(3) 0.029(2) 0.002(2) 0.004(2) -0.003(2) Li2 0.036(3) 0.059(4) 0.038(3) 0.017(2) -0.006(2) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C5 1.410(3) . ? O1 C6 1.422(4) . ? O1 Li2 2.375(6) . ? O2 C11 1.405(3) . ? O2 C12 1.424(4) . ? O2 Li2 2.389(6) . ? N1 C5 1.358(4) . ? N1 C1 1.465(4) . ? N1 Li2 2.033(6) . ? N1 Li1 2.067(5) . ? N2 C11 1.342(3) . ? N2 C7 1.452(4) . ? N2 Li2 2.002(6) . ? N2 Li1 2.075(5) . ? N3 C15 1.438(4) . ? N3 C14 1.462(4) . ? N3 C13 1.471(4) . ? N3 Li1 2.155(5) . ? N4 C18 1.448(5) . ? N4 C17 1.470(4) . ? N4 C16 1.485(5) . ? N4 Li1 2.201(5) . ? N5 C20 1.473(4) . ? N5 C19 1.479(4) . ? N5 C21 1.479(4) . ? N5 Li2 2.113(5) . ? C1 C2 1.511(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.528(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.502(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.347(4) . ? C4 H4 0.9500 . ? C5 Li2 2.589(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8B 1.377(15) . ? C7 C8A 1.470(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8A C9 1.521(5) . ? C8A H8A 0.9900 . ? C8A H8B 0.9900 . ? C8B C9 1.502(16) . ? C8B H8B1 0.9900 . ? C8B H8B2 0.9900 . ? C9 C10 1.506(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.352(4) . ? C10 H10 0.9500 . ? C11 Li2 2.617(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.496(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C21 1.500(6) 3_776 ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? Li1 Li2 2.444(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 O1 C6 117.5(2) . . ? C5 O1 Li2 82.1(2) . . ? C6 O1 Li2 150.3(2) . . ? C11 O2 C12 118.6(3) . . ? C11 O2 Li2 82.9(2) . . ? C12 O2 Li2 151.7(2) . . ? C5 N1 C1 111.2(2) . . ? C5 N1 Li2 97.6(2) . . ? C1 N1 Li2 127.0(2) . . ? C5 N1 Li1 115.5(2) . . ? C1 N1 Li1 125.1(2) . . ? Li2 N1 Li1 73.2(2) . . ? C11 N2 C7 111.4(2) . . ? C11 N2 Li2 101.1(2) . . ? C7 N2 Li2 129.5(3) . . ? C11 N2 Li1 117.1(2) . . ? C7 N2 Li1 119.3(2) . . ? Li2 N2 Li1 73.6(2) . . ? C15 N3 C14 110.9(3) . . ? C15 N3 C13 110.1(3) . . ? C14 N3 C13 108.4(3) . . ? C15 N3 Li1 106.5(2) . . ? C14 N3 Li1 105.7(2) . . ? C13 N3 Li1 115.1(2) . . ? C18 N4 C17 108.9(3) . . ? C18 N4 C16 111.8(3) . . ? C17 N4 C16 109.4(3) . . ? C18 N4 Li1 119.3(3) . . ? C17 N4 Li1 102.7(2) . . ? C16 N4 Li1 104.1(2) . . ? C20 N5 C19 108.7(3) . . ? C20 N5 C21 109.0(2) . . ? C19 N5 C21 111.0(2) . . ? C20 N5 Li2 102.6(2) . . ? C19 N5 Li2 109.8(2) . . ? C21 N5 Li2 115.3(2) . . ? N1 C1 C2 113.6(3) . . ? N1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C1 C2 C3 110.3(3) . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 110.3(3) . . ? C4 C3 H3A 109.6 . . ? C2 C3 H3A 109.6 . . ? C4 C3 H3B 109.6 . . ? C2 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 119.6(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 N1 129.7(3) . . ? C4 C5 O1 123.5(3) . . ? N1 C5 O1 106.8(2) . . ? C4 C5 Li2 152.2(2) . . ? N1 C5 Li2 51.11(18) . . ? O1 C5 Li2 65.28(19) . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8B C7 N2 123.9(6) . . ? C8B C7 C8A 36.4(9) . . ? N2 C7 C8A 115.9(3) . . ? C8B C7 H7A 125.4 . . ? N2 C7 H7A 108.3 . . ? C8A C7 H7A 108.3 . . ? C8B C7 H7B 72.4 . . ? N2 C7 H7B 108.3 . . ? C8A C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C7 C8A C9 111.8(3) . . ? C7 C8A H8A 109.3 . . ? C9 C8A H8A 109.3 . . ? C7 C8A H8B 109.3 . . ? C9 C8A H8B 109.3 . . ? H8A C8A H8B 107.9 . . ? C7 C8B C9 118.6(12) . . ? C7 C8B H8B1 107.7 . . ? C9 C8B H8B1 107.7 . . ? C7 C8B H8B2 107.7 . . ? C9 C8B H8B2 107.7 . . ? H8B1 C8B H8B2 107.1 . . ? C8B C9 C10 109.8(6) . . ? C8B C9 C8A 34.3(8) . . ? C10 C9 C8A 110.0(3) . . ? C8B C9 H9A 78.2 . . ? C10 C9 H9A 109.7 . . ? C8A C9 H9A 109.7 . . ? C8B C9 H9B 134.7 . . ? C10 C9 H9B 109.7 . . ? C8A C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 118.7(3) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? N2 C11 C10 130.3(3) . . ? N2 C11 O2 107.2(3) . . ? C10 C11 O2 122.5(3) . . ? N2 C11 Li2 48.66(18) . . ? C10 C11 Li2 156.4(2) . . ? O2 C11 Li2 64.95(19) . . ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 111.9(3) . . ? N3 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N3 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? N4 C16 C15 112.4(3) . . ? N4 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? N4 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? N4 C17 H17A 109.5 . . ? N4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 H18A 109.5 . . ? N4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 H19A 109.5 . . ? N5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N5 C20 H20A 109.5 . . ? N5 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N5 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 C21 112.7(3) . 3_776 ? N5 C21 H21A 109.0 . . ? C21 C21 H21A 109.0 3_776 . ? N5 C21 H21B 109.0 . . ? C21 C21 H21B 109.0 3_776 . ? H21A C21 H21B 107.8 . . ? N1 Li1 N2 104.5(2) . . ? N1 Li1 N3 120.8(3) . . ? N2 Li1 N3 112.4(2) . . ? N1 Li1 N4 112.5(2) . . ? N2 Li1 N4 123.7(3) . . ? N3 Li1 N4 83.02(18) . . ? N1 Li1 Li2 52.78(17) . . ? N2 Li1 Li2 51.81(17) . . ? N3 Li1 Li2 139.2(3) . . ? N4 Li1 Li2 137.7(3) . . ? N2 Li2 N1 108.5(2) . . ? N2 Li2 N5 133.2(3) . . ? N1 Li2 N5 118.3(3) . . ? N2 Li2 O1 103.1(2) . . ? N1 Li2 O1 59.97(16) . . ? N5 Li2 O1 100.3(2) . . ? N2 Li2 O2 59.69(16) . . ? N1 Li2 O2 101.5(2) . . ? N5 Li2 O2 108.1(2) . . ? O1 Li2 O2 151.3(2) . . ? N2 Li2 Li1 54.56(18) . . ? N1 Li2 Li1 54.04(17) . . ? N5 Li2 Li1 172.0(3) . . ? O1 Li2 Li1 74.05(18) . . ? O2 Li2 Li1 77.29(19) . . ? N2 Li2 C5 120.0(2) . . ? N1 Li2 C5 31.33(12) . . ? N5 Li2 C5 101.2(2) . . ? O1 Li2 C5 32.63(10) . . ? O2 Li2 C5 132.8(2) . . ? Li1 Li2 C5 70.89(18) . . ? N2 Li2 C11 30.22(11) . . ? N1 Li2 C11 117.0(2) . . ? N5 Li2 C11 116.8(2) . . ? O1 Li2 C11 133.2(2) . . ? O2 Li2 C11 32.20(10) . . ? Li1 Li2 C11 70.95(18) . . ? C5 Li2 C11 141.8(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.313 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.054 data_cmp3 _database_code_depnum_ccdc_archive 'CCDC 764916' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H70 Li8 N8 O7' _chemical_formula_sum 'C46 H70 Li8 N8 O7' _chemical_formula_weight 902.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.745(2) _cell_length_b 11.472(2) _cell_length_c 12.207(2) _cell_angle_alpha 69.40(3) _cell_angle_beta 64.82(3) _cell_angle_gamma 82.48(3) _cell_volume 1274.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 482 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16315 _diffrn_reflns_av_R_equivalents 0.1158 _diffrn_reflns_av_sigmaI/netI 0.0921 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4470 _reflns_number_gt 3237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'CIFTAB (Shelrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1186P)^2^+0.0511P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4470 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.1916 _refine_ls_wR_factor_gt 0.1709 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.18844(17) 0.20017(19) -0.03700(16) 0.0350(5) Uani 1 1 d . . . O2 O -0.31160(16) 0.10838(15) 0.13913(16) 0.0261(4) Uani 1 1 d . . . O3 O 0.00353(17) -0.00722(15) -0.24318(14) 0.0226(4) Uani 1 1 d . . . O4 O 0.0000 0.0000 0.0000 0.0181(5) Uani 1 2 d S . . N1 N 0.1301(2) 0.27078(19) -0.20709(18) 0.0219(5) Uani 1 1 d . . . N2 N -0.1481(2) 0.25039(18) 0.07964(19) 0.0231(5) Uani 1 1 d . . . N3 N -0.1581(2) 0.12420(18) -0.16659(18) 0.0222(5) Uani 1 1 d . . . N4 N -0.1363(2) 0.48159(19) -0.1985(2) 0.0291(5) Uani 1 1 d . . . C1 C 0.1796(3) 0.3034(2) -0.3470(2) 0.0281(6) Uani 1 1 d . . . H1A H 0.1039 0.3423 -0.3724 0.034 Uiso 1 1 calc R . . H1B H 0.2036 0.2260 -0.3692 0.034 Uiso 1 1 calc R . . C2 C 0.3028(3) 0.3911(3) -0.4231(3) 0.0325(7) Uani 1 1 d . . . H2A H 0.2805 0.4694 -0.4024 0.039 Uiso 1 1 calc R . . H2B H 0.3285 0.4117 -0.5160 0.039 Uiso 1 1 calc R . . C3 C 0.4233(3) 0.3282(3) -0.3896(3) 0.0370(7) Uani 1 1 d . . . H3A H 0.4625 0.2645 -0.4319 0.044 Uiso 1 1 calc R . . H3B H 0.4964 0.3910 -0.4211 0.044 Uiso 1 1 calc R . . C4 C 0.3731(2) 0.2681(2) -0.2464(2) 0.0266(6) Uani 1 1 d . . . H4 H 0.4375 0.2429 -0.2085 0.032 Uiso 1 1 calc R . . C5 C 0.2382(2) 0.2499(2) -0.1722(2) 0.0205(6) Uani 1 1 d . . . C6 C 0.2766(3) 0.2068(3) 0.0212(2) 0.0338(7) Uani 1 1 d . . . H6A H 0.3517 0.1484 0.0033 0.051 Uiso 1 1 calc R . . H6B H 0.2238 0.1849 0.1141 0.051 Uiso 1 1 calc R . . H6C H 0.3147 0.2917 -0.0138 0.051 Uiso 1 1 calc R . . C7 C -0.1033(3) 0.3437(2) 0.1144(3) 0.0293(6) Uani 1 1 d . . . H7A H -0.0210 0.3891 0.0404 0.035 Uiso 1 1 calc R . . H7B H -0.0762 0.2996 0.1864 0.035 Uiso 1 1 calc R . . C8 C -0.2117(3) 0.4372(2) 0.1528(2) 0.0295(6) Uani 1 1 d . . . H8A H -0.1742 0.4976 0.1730 0.035 Uiso 1 1 calc R . . H8B H -0.2383 0.4838 0.0809 0.035 Uiso 1 1 calc R . . C9 C -0.3366(3) 0.3700(2) 0.2692(3) 0.0316(6) Uani 1 1 d . . . H9A H -0.3181 0.3462 0.3469 0.038 Uiso 1 1 calc R . . H9B H -0.4160 0.4260 0.2799 0.038 Uiso 1 1 calc R . . C10 C -0.3705(2) 0.2547(2) 0.2535(2) 0.0254(6) Uani 1 1 d . . . H10 H -0.4565 0.2124 0.3094 0.030 Uiso 1 1 calc R . . C11 C -0.2800(2) 0.2118(2) 0.1613(2) 0.0208(6) Uani 1 1 d . . . C12 C -0.4526(3) 0.0660(3) 0.2016(3) 0.0450(8) Uani 1 1 d . . . H12A H -0.4811 0.0357 0.2948 0.067 Uiso 1 1 calc R . . H12B H -0.4622 -0.0017 0.1741 0.067 Uiso 1 1 calc R . . H12C H -0.5108 0.1351 0.1787 0.067 Uiso 1 1 calc R . . C13 C -0.2800(3) 0.1954(2) -0.1722(2) 0.0251(6) Uani 1 1 d . . . H13A H -0.3023 0.2508 -0.1202 0.030 Uiso 1 1 calc R . . H13B H -0.3591 0.1371 -0.1344 0.030 Uiso 1 1 calc R . . C14 C -0.2595(3) 0.2740(2) -0.3092(2) 0.0280(6) Uani 1 1 d . . . H14A H -0.3408 0.3261 -0.3081 0.034 Uiso 1 1 calc R . . H14B H -0.1778 0.3298 -0.3497 0.034 Uiso 1 1 calc R . . C15 C -0.2397(3) 0.1879(3) -0.3856(2) 0.0321(7) Uani 1 1 d . . . H15A H -0.3291 0.1495 -0.3610 0.038 Uiso 1 1 calc R . . H15B H -0.2030 0.2360 -0.4783 0.038 Uiso 1 1 calc R . . C16 C -0.1404(3) 0.0876(2) -0.3584(2) 0.0268(6) Uani 1 1 d . . . H16 H -0.1027 0.0356 -0.4101 0.032 Uiso 1 1 calc R . . C17 C -0.1056(2) 0.0723(2) -0.2609(2) 0.0210(6) Uani 1 1 d . . . C18 C 0.0990(3) -0.0424(2) -0.3504(2) 0.0289(6) Uani 1 1 d . . . H18A H 0.0542 -0.1018 -0.3642 0.043 Uiso 1 1 calc R . . H18B H 0.1785 -0.0813 -0.3331 0.043 Uiso 1 1 calc R . . H18C H 0.1297 0.0317 -0.4272 0.043 Uiso 1 1 calc R . . C19 C -0.2711(3) 0.5032(2) -0.1499(3) 0.0303(6) Uani 1 1 d . . . H19 H -0.3291 0.4442 -0.0721 0.036 Uiso 1 1 calc R . . C20 C -0.3300(3) 0.6069(3) -0.2071(3) 0.0351(7) Uani 1 1 d . . . H20 H -0.4264 0.6187 -0.1701 0.042 Uiso 1 1 calc R . . C21 C -0.2467(3) 0.6924(3) -0.3185(3) 0.0361(7) Uani 1 1 d . . . H21 H -0.2848 0.7644 -0.3603 0.043 Uiso 1 1 calc R . . C22 C -0.1077(3) 0.6738(3) -0.3696(3) 0.0318(6) Uani 1 1 d . . . H22 H -0.0480 0.7330 -0.4461 0.038 Uiso 1 1 calc R . . C23 C -0.0571(3) 0.5670(2) -0.3072(2) 0.0288(6) Uani 1 1 d . . . H23 H 0.0389 0.5535 -0.3432 0.035 Uiso 1 1 calc R . . Li1 Li -0.0602(5) 0.3189(4) -0.1130(4) 0.0398(12) Uani 1 1 d . . . Li2 Li 0.0028(4) 0.1238(4) 0.0645(4) 0.0217(9) Uani 1 1 d . . . Li3 Li -0.1774(4) 0.0387(4) 0.0142(4) 0.0259(9) Uani 1 1 d . . . Li4 Li -0.0347(4) -0.1113(4) 0.1604(4) 0.0242(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0225(10) 0.0628(13) 0.0164(10) -0.0037(9) -0.0092(8) -0.0103(9) O2 0.0207(9) 0.0236(10) 0.0321(10) -0.0146(8) -0.0048(8) 0.0004(7) O3 0.0291(10) 0.0270(10) 0.0162(9) -0.0112(7) -0.0124(8) 0.0088(8) O4 0.0212(12) 0.0183(12) 0.0177(12) -0.0087(10) -0.0097(10) 0.0059(10) N1 0.0185(11) 0.0284(12) 0.0162(11) -0.0054(9) -0.0060(9) -0.0010(9) N2 0.0213(11) 0.0175(11) 0.0232(12) -0.0082(9) -0.0023(9) 0.0036(9) N3 0.0235(11) 0.0248(12) 0.0221(11) -0.0094(9) -0.0133(9) 0.0070(9) N4 0.0260(12) 0.0252(12) 0.0296(13) -0.0039(10) -0.0103(11) 0.0030(10) C1 0.0284(15) 0.0317(15) 0.0218(14) -0.0072(12) -0.0099(12) 0.0026(12) C2 0.0332(16) 0.0346(16) 0.0235(14) -0.0034(12) -0.0104(13) -0.0011(13) C3 0.0225(15) 0.0479(18) 0.0264(15) -0.0048(13) -0.0023(12) -0.0016(13) C4 0.0186(13) 0.0317(15) 0.0253(14) -0.0057(12) -0.0090(12) 0.0036(11) C5 0.0223(14) 0.0184(13) 0.0200(13) -0.0061(10) -0.0084(11) 0.0009(10) C6 0.0329(15) 0.0465(18) 0.0273(15) -0.0112(13) -0.0160(13) -0.0061(13) C7 0.0258(14) 0.0173(14) 0.0341(15) -0.0054(11) -0.0040(12) -0.0028(11) C8 0.0340(16) 0.0226(14) 0.0291(15) -0.0113(12) -0.0081(13) 0.0010(12) C9 0.0315(15) 0.0331(16) 0.0308(15) -0.0179(13) -0.0083(13) 0.0037(12) C10 0.0167(13) 0.0297(15) 0.0258(14) -0.0124(12) -0.0027(11) 0.0014(11) C11 0.0221(13) 0.0164(13) 0.0230(13) -0.0065(11) -0.0093(11) 0.0040(10) C12 0.0243(15) 0.0451(19) 0.070(2) -0.0371(17) -0.0085(15) -0.0022(13) C13 0.0239(13) 0.0261(14) 0.0263(14) -0.0059(11) -0.0140(12) 0.0028(11) C14 0.0230(14) 0.0257(14) 0.0352(15) -0.0023(12) -0.0189(12) 0.0031(11) C15 0.0292(15) 0.0421(17) 0.0243(15) -0.0012(12) -0.0174(12) -0.0023(13) C16 0.0323(15) 0.0305(15) 0.0218(14) -0.0080(11) -0.0155(12) 0.0013(12) C17 0.0220(13) 0.0198(13) 0.0204(13) -0.0027(10) -0.0111(11) 0.0002(10) C18 0.0347(15) 0.0325(15) 0.0195(14) -0.0132(12) -0.0099(12) 0.0102(12) C19 0.0309(15) 0.0275(15) 0.0280(15) -0.0090(12) -0.0084(12) 0.0021(12) C20 0.0279(15) 0.0413(18) 0.0357(17) -0.0146(14) -0.0137(14) 0.0104(13) C21 0.0380(17) 0.0335(16) 0.0342(17) -0.0067(13) -0.0196(14) 0.0140(13) C22 0.0339(16) 0.0274(15) 0.0264(15) -0.0005(12) -0.0122(13) 0.0009(12) C23 0.0240(14) 0.0268(15) 0.0311(15) -0.0048(12) -0.0115(12) 0.0029(11) Li1 0.027(2) 0.039(3) 0.026(3) 0.004(2) -0.002(2) 0.014(2) Li2 0.023(2) 0.024(2) 0.020(2) -0.0114(18) -0.0084(18) 0.0048(17) Li3 0.024(2) 0.029(2) 0.024(2) -0.0086(19) -0.0096(19) 0.0006(18) Li4 0.030(2) 0.027(2) 0.021(2) -0.0103(18) -0.0141(19) 0.0023(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C5 1.414(3) . ? O1 C6 1.427(3) . ? O1 Li2 1.967(4) . ? O1 Li3 2.668(5) 2 ? O2 C11 1.416(3) . ? O2 C12 1.436(3) . ? O2 Li3 1.931(4) . ? O3 C18 1.431(3) . ? O3 C17 1.433(3) . ? O3 Li4 2.087(4) 2 ? O3 Li2 2.096(4) 2 ? O4 Li4 1.830(4) 2 ? O4 Li4 1.830(4) . ? O4 Li3 1.847(4) . ? O4 Li3 1.847(4) 2 ? O4 Li2 1.860(4) . ? O4 Li2 1.860(4) 2 ? N1 C5 1.365(3) . ? N1 C1 1.472(3) . ? N1 Li1 1.990(5) . ? N1 Li4 1.996(5) 2 ? N2 C11 1.360(3) . ? N2 C7 1.478(3) . ? N2 Li1 2.010(5) . ? N2 Li2 2.023(4) . ? N3 C17 1.356(3) . ? N3 C13 1.464(3) . ? N3 Li3 2.004(5) . ? N3 Li4 2.089(4) 2 ? N4 C23 1.337(3) . ? N4 C19 1.338(3) . ? N4 Li1 2.049(5) . ? C1 C2 1.507(4) . ? C1 Li4 2.610(5) 2 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.536(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.507(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.339(3) . ? C4 H4 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.514(4) . ? C7 Li1 2.725(6) . ? C7 Li2 2.787(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.513(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.510(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.337(3) . ? C10 H10 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.528(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.522(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.512(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.342(3) . ? C16 H16 0.9500 . ? C17 Li4 2.472(4) 2 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.378(4) . ? C19 H19 0.9500 . ? C20 C21 1.366(4) . ? C20 H20 0.9500 . ? C21 C22 1.372(4) . ? C21 H21 0.9500 . ? C22 C23 1.378(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? Li1 Li4 2.622(6) 2 ? Li1 Li2 2.757(6) . ? Li1 Li3 3.196(7) . ? Li2 O3 2.096(4) 2 ? Li2 Li4 2.544(6) . ? Li2 Li3 2.594(6) 2 ? Li2 Li3 2.647(5) . ? Li2 Li4 2.673(5) 2 ? Li3 Li4 2.355(6) 2 ? Li3 Li2 2.594(6) 2 ? Li3 O1 2.668(5) 2 ? Li3 Li4 2.824(6) . ? Li4 N1 1.996(5) 2 ? Li4 O3 2.087(4) 2 ? Li4 N3 2.089(4) 2 ? Li4 Li3 2.355(6) 2 ? Li4 C17 2.472(4) 2 ? Li4 C1 2.610(5) 2 ? Li4 Li1 2.622(6) 2 ? Li4 Li2 2.673(5) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 O1 C6 118.11(18) . . ? C5 O1 Li2 119.76(17) . . ? C6 O1 Li2 122.12(18) . . ? C5 O1 Li3 97.50(16) . 2 ? C6 O1 Li3 106.26(18) . 2 ? Li2 O1 Li3 66.05(15) . 2 ? C11 O2 C12 117.32(18) . . ? C11 O2 Li3 122.02(18) . . ? C12 O2 Li3 120.23(18) . . ? C18 O3 C17 117.16(18) . . ? C18 O3 Li4 128.94(18) . 2 ? C17 O3 Li4 87.15(16) . 2 ? C18 O3 Li2 114.90(18) . 2 ? C17 O3 Li2 124.35(17) . 2 ? Li4 O3 Li2 74.91(16) 2 2 ? Li4 O4 Li4 180.0(4) 2 . ? Li4 O4 Li3 79.64(19) 2 . ? Li4 O4 Li3 100.36(19) . . ? Li4 O4 Li3 100.36(19) 2 2 ? Li4 O4 Li3 79.64(19) . 2 ? Li3 O4 Li3 180.0(5) . 2 ? Li4 O4 Li2 92.82(17) 2 . ? Li4 O4 Li2 87.18(17) . . ? Li3 O4 Li2 91.17(17) . . ? Li3 O4 Li2 88.83(17) 2 . ? Li4 O4 Li2 87.18(17) 2 2 ? Li4 O4 Li2 92.82(17) . 2 ? Li3 O4 Li2 88.83(17) . 2 ? Li3 O4 Li2 91.17(17) 2 2 ? Li2 O4 Li2 180.0(2) . 2 ? C5 N1 C1 110.62(19) . . ? C5 N1 Li1 128.4(2) . . ? C1 N1 Li1 117.2(2) . . ? C5 N1 Li4 111.1(2) . 2 ? C1 N1 Li4 96.49(18) . 2 ? Li1 N1 Li4 82.3(2) . 2 ? C11 N2 C7 110.43(19) . . ? C11 N2 Li1 130.4(2) . . ? C7 N2 Li1 101.6(2) . . ? C11 N2 Li2 119.30(19) . . ? C7 N2 Li2 104.46(18) . . ? Li1 N2 Li2 86.24(18) . . ? C17 N3 C13 109.85(19) . . ? C17 N3 Li3 125.1(2) . . ? C13 N3 Li3 112.06(19) . . ? C17 N3 Li4 89.10(17) . 2 ? C13 N3 Li4 150.77(19) . 2 ? Li3 N3 Li4 70.20(17) . 2 ? C23 N4 C19 117.0(2) . . ? C23 N4 Li1 122.6(2) . . ? C19 N4 Li1 120.3(2) . . ? N1 C1 C2 114.0(2) . . ? N1 C1 Li4 49.43(13) . 2 ? C2 C1 Li4 154.6(2) . 2 ? N1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? Li4 C1 H1A 95.8 2 . ? N1 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? Li4 C1 H1B 67.9 2 . ? H1A C1 H1B 107.6 . . ? C1 C2 C3 109.0(2) . . ? C1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C4 C3 C2 109.6(2) . . ? C4 C3 H3A 109.8 . . ? C2 C3 H3A 109.8 . . ? C4 C3 H3B 109.8 . . ? C2 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C3 120.4(2) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 N1 129.2(2) . . ? C4 C5 O1 121.3(2) . . ? N1 C5 O1 109.46(19) . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 114.1(2) . . ? N2 C7 Li1 46.27(15) . . ? C8 C7 Li1 113.8(2) . . ? N2 C7 Li2 44.64(13) . . ? C8 C7 Li2 157.36(19) . . ? Li1 C7 Li2 60.00(14) . . ? N2 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? Li1 C7 H7A 65.3 . . ? Li2 C7 H7A 88.9 . . ? N2 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? Li1 C7 H7B 136.8 . . ? Li2 C7 H7B 77.9 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 109.6(2) . . ? C9 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? C9 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 110.1(2) . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 120.3(2) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 N2 129.4(2) . . ? C10 C11 O2 121.8(2) . . ? N2 C11 O2 108.83(19) . . ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 112.5(2) . . ? N3 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N3 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 109.0(2) . . ? C15 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? C15 C14 H14B 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C16 C15 C14 109.1(2) . . ? C16 C15 H15A 109.9 . . ? C14 C15 H15A 109.9 . . ? C16 C15 H15B 109.9 . . ? C14 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C17 C16 C15 119.7(2) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 N3 130.1(2) . . ? C16 C17 O3 121.9(2) . . ? N3 C17 O3 107.96(18) . . ? C16 C17 Li4 154.8(2) . 2 ? N3 C17 Li4 57.65(15) . 2 ? O3 C17 Li4 57.48(14) . 2 ? O3 C18 H18A 109.5 . . ? O3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 C20 123.2(3) . . ? N4 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C21 C20 C19 118.5(3) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C20 C21 C22 119.7(3) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 118.3(3) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? N4 C23 C22 123.3(3) . . ? N4 C23 H23 118.3 . . ? C22 C23 H23 118.3 . . ? N1 Li1 N2 119.6(2) . . ? N1 Li1 N4 119.5(2) . . ? N2 Li1 N4 116.8(2) . . ? N1 Li1 Li4 48.95(15) . 2 ? N2 Li1 Li4 99.0(2) . 2 ? N4 Li1 Li4 137.0(3) . 2 ? N1 Li1 C7 113.9(2) . . ? N2 Li1 C7 32.09(11) . . ? N4 Li1 C7 102.1(2) . . ? Li4 Li1 C7 120.6(2) 2 . ? N1 Li1 Li2 73.90(17) . . ? N2 Li1 Li2 47.06(13) . . ? N4 Li1 Li2 162.8(3) . . ? Li4 Li1 Li2 59.52(15) 2 . ? C7 Li1 Li2 61.12(14) . . ? N1 Li1 Li3 93.5(2) . . ? N2 Li1 Li3 62.96(15) . . ? N4 Li1 Li3 131.5(2) . . ? Li4 Li1 Li3 46.46(14) 2 . ? C7 Li1 Li3 94.28(16) . . ? Li2 Li1 Li3 52.18(13) . . ? O4 Li2 O1 105.52(19) . . ? O4 Li2 N2 118.9(2) . . ? O1 Li2 N2 113.1(2) . . ? O4 Li2 O3 97.69(18) . 2 ? O1 Li2 O3 107.28(19) . 2 ? N2 Li2 O3 112.77(19) . 2 ? O4 Li2 Li4 45.93(12) . . ? O1 Li2 Li4 121.6(2) . . ? N2 Li2 Li4 125.2(2) . . ? O3 Li2 Li4 52.38(13) 2 . ? O4 Li2 Li3 45.38(12) . 2 ? O1 Li2 Li3 70.08(16) . 2 ? N2 Li2 Li3 161.5(2) . 2 ? O3 Li2 Li3 82.10(17) 2 2 ? Li4 Li2 Li3 54.54(15) . 2 ? O4 Li2 Li3 44.22(12) . . ? O1 Li2 Li3 135.2(2) . . ? N2 Li2 Li3 75.47(16) . . ? O3 Li2 Li3 108.83(19) 2 . ? Li4 Li2 Li3 65.87(16) . . ? Li3 Li2 Li3 89.60(17) 2 . ? O4 Li2 Li4 43.15(12) . 2 ? O1 Li2 Li4 82.71(16) . 2 ? N2 Li2 Li4 97.06(18) . 2 ? O3 Li2 Li4 140.1(2) 2 2 ? Li4 Li2 Li4 89.08(17) . 2 ? Li3 Li2 Li4 64.83(15) 2 2 ? Li3 Li2 Li4 52.54(15) . 2 ? O4 Li2 Li1 96.92(19) . . ? O1 Li2 Li1 82.85(18) . . ? N2 Li2 Li1 46.69(14) . . ? O3 Li2 Li1 159.2(2) 2 . ? Li4 Li2 Li1 137.5(2) . . ? Li3 Li2 Li1 118.69(19) 2 . ? Li3 Li2 Li1 72.47(18) . . ? Li4 Li2 Li1 57.74(16) 2 . ? O4 Li2 C7 149.2(2) . . ? O1 Li2 C7 90.91(16) . . ? N2 Li2 C7 30.90(9) . . ? O3 Li2 C7 102.02(15) 2 . ? Li4 Li2 C7 141.81(19) . . ? Li3 Li2 C7 160.83(19) 2 . ? Li3 Li2 C7 106.37(17) . . ? Li4 Li2 C7 116.61(18) 2 . ? Li1 Li2 C7 58.88(15) . . ? O4 Li3 O2 124.7(2) . . ? O4 Li3 N3 104.8(2) . . ? O2 Li3 N3 115.2(2) . . ? O4 Li3 Li4 49.87(14) . 2 ? O2 Li3 Li4 133.9(2) . 2 ? N3 Li3 Li4 56.58(15) . 2 ? O4 Li3 Li2 45.79(12) . 2 ? O2 Li3 Li2 156.0(2) . 2 ? N3 Li3 Li2 88.44(18) . 2 ? Li4 Li3 Li2 61.65(17) 2 2 ? O4 Li3 Li2 44.61(12) . . ? O2 Li3 Li2 84.18(16) . . ? N3 Li3 Li2 112.5(2) . . ? Li4 Li3 Li2 64.28(16) 2 . ? Li2 Li3 Li2 90.40(17) 2 . ? O4 Li3 O1 82.74(16) . 2 ? O2 Li3 O1 122.0(2) . 2 ? N3 Li3 O1 101.38(17) . 2 ? Li4 Li3 O1 103.46(18) 2 2 ? Li2 Li3 O1 43.87(12) 2 2 ? Li2 Li3 O1 122.01(19) . 2 ? O4 Li3 Li4 39.60(12) . . ? O2 Li3 Li4 99.53(18) . . ? N3 Li3 Li4 142.5(2) . . ? Li4 Li3 Li4 89.47(19) 2 . ? Li2 Li3 Li4 58.93(14) 2 . ? Li2 Li3 Li4 55.30(15) . . ? O1 Li3 Li4 68.94(14) 2 . ? O4 Li3 Li1 83.53(16) . . ? O2 Li3 Li1 80.96(17) . . ? N3 Li3 Li1 64.69(15) . . ? Li4 Li3 Li1 53.84(16) 2 . ? Li2 Li3 Li1 114.83(18) 2 . ? Li2 Li3 Li1 55.35(15) . . ? O1 Li3 Li1 157.04(18) 2 . ? Li4 Li3 Li1 110.16(17) . . ? O4 Li4 N1 116.56(19) . 2 ? O4 Li4 O3 98.97(19) . 2 ? N1 Li4 O3 141.4(2) 2 2 ? O4 Li4 N3 102.1(2) . 2 ? N1 Li4 N3 117.1(2) 2 2 ? O3 Li4 N3 65.39(13) 2 2 ? O4 Li4 Li3 50.49(15) . 2 ? N1 Li4 Li3 125.2(2) 2 2 ? O3 Li4 Li3 88.41(18) 2 2 ? N3 Li4 Li3 53.22(15) 2 2 ? O4 Li4 C17 113.63(19) . 2 ? N1 Li4 C17 126.8(2) 2 2 ? O3 Li4 C17 35.37(9) 2 2 ? N3 Li4 C17 33.25(10) 2 2 ? Li3 Li4 C17 76.72(16) 2 2 ? O4 Li4 Li2 46.89(13) . . ? N1 Li4 Li2 154.2(2) 2 . ? O3 Li4 Li2 52.71(13) 2 . ? N3 Li4 Li2 88.00(18) 2 . ? Li3 Li4 Li2 63.81(17) 2 . ? C17 Li4 Li2 77.38(15) 2 . ? O4 Li4 C1 147.3(2) . 2 ? N1 Li4 C1 34.08(10) 2 2 ? O3 Li4 C1 107.42(17) 2 2 ? N3 Li4 C1 106.14(18) 2 2 ? Li3 Li4 C1 146.5(2) 2 2 ? C17 Li4 C1 99.02(16) 2 2 ? Li2 Li4 C1 148.6(2) . 2 ? O4 Li4 Li1 102.43(19) . 2 ? N1 Li4 Li1 48.75(15) 2 2 ? O3 Li4 Li1 139.7(2) 2 2 ? N3 Li4 Li1 76.88(18) 2 2 ? Li3 Li4 Li1 79.70(19) 2 2 ? C17 Li4 Li1 104.4(2) 2 2 ? Li2 Li4 Li1 142.3(2) . 2 ? C1 Li4 Li1 69.08(15) 2 2 ? O4 Li4 Li2 44.03(12) . 2 ? N1 Li4 Li2 75.84(15) 2 2 ? O3 Li4 Li2 142.2(2) 2 2 ? N3 Li4 Li2 108.73(19) 2 2 ? Li3 Li4 Li2 63.18(16) 2 2 ? C17 Li4 Li2 139.2(2) 2 2 ? Li2 Li4 Li2 90.92(17) . 2 ? C1 Li4 Li2 109.89(17) 2 2 ? Li1 Li4 Li2 62.74(16) 2 2 ? O4 Li4 Li3 40.04(12) . . ? N1 Li4 Li3 95.65(17) 2 . ? O3 Li4 Li3 103.02(18) 2 . ? N3 Li4 Li3 140.5(2) 2 . ? Li3 Li4 Li3 90.53(19) 2 . ? C17 Li4 Li3 135.31(19) 2 . ? Li2 Li4 Li3 58.82(15) . . ? C1 Li4 Li3 113.32(17) 2 . ? Li1 Li4 Li3 115.35(19) 2 . ? Li2 Li4 Li3 56.24(14) 2 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.647 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.092 data_mag _database_code_depnum_ccdc_archive 'CCDC 764917' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H78 Li6 N8 O6, C6 H14' _chemical_formula_sum 'C44 H92 Li6 N8 O6' _chemical_formula_weight 870.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.235(4) _cell_length_b 15.067(3) _cell_length_c 18.853(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.41(3) _cell_angle_gamma 90.00 _cell_volume 5421.2(22) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 23100 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.76 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23100 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4767 _reflns_number_gt 3354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+3.2270P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4767 _refine_ls_number_parameters 344 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1290 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.14135(9) 0.36258(9) 0.33565(9) 0.0487(4) Uani 1 1 d . . . N1 N 0.19747(9) 0.48803(11) 0.33211(9) 0.0360(4) Uani 1 1 d . . . C1 C 0.26388(12) 0.53728(16) 0.35766(12) 0.0477(6) Uani 1 1 d . . . H1A H 0.2550 0.5993 0.3396 0.057 Uiso 1 1 calc R . . H1B H 0.2965 0.5106 0.3345 0.057 Uiso 1 1 calc R . . Li1 Li 0.15185(18) 0.4702(2) 0.22045(19) 0.0351(8) Uani 1 1 d . . . O2 O 0.05851(7) 0.52167(8) 0.20333(7) 0.0297(3) Uani 1 1 d . . . N2 N 0.15319(10) 0.35135(11) 0.16225(9) 0.0406(5) Uani 1 1 d . . . C2 C 0.29860(14) 0.5382(2) 0.44180(14) 0.0616(7) Uani 1 1 d . . . H2A H 0.2671 0.5662 0.4658 0.074 Uiso 1 1 calc R . . H2B H 0.3424 0.5732 0.4553 0.074 Uiso 1 1 calc R . . Li2 Li 0.09919(18) 0.5378(2) 0.31258(19) 0.0369(8) Uani 1 1 d . . . O3 O 0.06935(7) 0.65998(8) 0.30914(7) 0.0358(4) Uani 1 1 d D . . N3 N 0.20045(9) 0.52950(12) 0.14238(9) 0.0392(4) Uani 1 1 d . A . C3 C 0.31495(14) 0.4431(2) 0.46991(14) 0.0689(8) Uani 1 1 d . . . H3A H 0.3569 0.4218 0.4590 0.083 Uiso 1 1 calc R . . H3B H 0.3254 0.4415 0.5251 0.083 Uiso 1 1 calc R . . Li3 Li 0.02936(18) 0.6468(2) 0.19949(18) 0.0349(8) Uani 1 1 d . . . N4 N 0.07701(10) 0.71867(11) 0.13257(9) 0.0399(4) Uani 1 1 d . . . C4 C 0.25418(14) 0.38327(18) 0.43259(13) 0.0556(7) Uani 1 1 d . . . H4 H 0.2521 0.3257 0.4523 0.067 Uiso 1 1 calc R . . C5 C 0.20240(11) 0.41142(14) 0.37081(12) 0.0386(5) Uani 1 1 d . . . C6 C 0.12938(17) 0.28460(16) 0.37256(17) 0.0726(9) Uani 1 1 d . . . H6A H 0.1670 0.2418 0.3773 0.109 Uiso 1 1 calc R . . H6B H 0.0843 0.2583 0.3431 0.109 Uiso 1 1 calc R . . H6C H 0.1285 0.3002 0.4227 0.109 Uiso 1 1 calc R . . C7 C 0.08712(15) 0.80516(15) 0.17139(14) 0.0546(7) Uani 1 1 d . A . H7A H 0.1162 0.8434 0.1518 0.082 Uiso 1 1 calc R . . H7B H 0.1104 0.7962 0.2255 0.082 Uiso 1 1 calc R . . H7C H 0.0415 0.8334 0.1627 0.082 Uiso 1 1 calc R . . C8 C 0.04254(14) 0.73333(16) 0.05154(12) 0.0527(6) Uani 1 1 d . A . H8A H -0.0017 0.7651 0.0432 0.079 Uiso 1 1 calc R . . H8B H 0.0330 0.6760 0.0256 0.079 Uiso 1 1 calc R . . H8C H 0.0733 0.7686 0.0319 0.079 Uiso 1 1 calc R . . C9 C 0.14619(12) 0.67691(14) 0.14895(12) 0.0405(5) Uani 1 1 d . A . H9A H 0.1645 0.6613 0.2030 0.049 Uiso 1 1 calc R . . H9B H 0.1787 0.7206 0.1393 0.049 Uiso 1 1 calc R . . C10 C 0.14571(12) 0.59329(14) 0.10257(11) 0.0398(5) Uani 1 1 d . . . H10A H 0.0993 0.5642 0.0900 0.048 Uiso 1 1 calc R A . H10B H 0.1526 0.6106 0.0548 0.048 Uiso 1 1 calc R . . C11 C 0.26966(13) 0.57223(18) 0.16691(14) 0.0551(6) Uani 1 1 d . . . H11A H 0.2788 0.5976 0.1232 0.083 Uiso 1 1 calc R A . H11B H 0.3057 0.5281 0.1910 0.083 Uiso 1 1 calc R . . H11C H 0.2706 0.6195 0.2029 0.083 Uiso 1 1 calc R . . C12 C 0.20201(13) 0.45480(15) 0.09108(13) 0.0482(6) Uani 1 1 d . . . H12A H 0.2493 0.4278 0.1083 0.058 Uiso 1 1 calc R A . H12B H 0.1936 0.4787 0.0399 0.058 Uiso 1 1 calc R . . C13 C 0.14875(13) 0.38399(14) 0.08733(12) 0.0468(6) Uani 1 1 d . A . H13A H 0.1012 0.4081 0.0619 0.056 Uiso 1 1 calc R . . H13B H 0.1560 0.3338 0.0569 0.056 Uiso 1 1 calc R . . C14 C 0.22250(13) 0.31671(17) 0.20549(14) 0.0547(7) Uani 1 1 d . . . H14A H 0.2369 0.2726 0.1753 0.082 Uiso 1 1 calc R . . H14B H 0.2205 0.2889 0.2517 0.082 Uiso 1 1 calc R . . H14C H 0.2565 0.3655 0.2183 0.082 Uiso 1 1 calc R . . C15 C 0.10093(14) 0.28084(14) 0.15339(14) 0.0552(7) Uani 1 1 d . . . H15A H 0.0546 0.3029 0.1230 0.083 Uiso 1 1 calc R . . H15B H 0.1000 0.2629 0.2030 0.083 Uiso 1 1 calc R . . H15C H 0.1134 0.2297 0.1283 0.083 Uiso 1 1 calc R . . C16 C 0.00718(10) 0.46989(12) 0.16243(11) 0.0314(5) Uani 1 1 d . . . H16 H 0.0035 0.4131 0.1826 0.038 Uiso 1 1 calc R . . C17 C -0.03992(11) 0.48933(15) 0.09575(11) 0.0394(5) Uani 1 1 d . . . H17A H -0.0385 0.5453 0.0731 0.047 Uiso 1 1 calc R . . H17B H -0.0749 0.4472 0.0709 0.047 Uiso 1 1 calc R . . C18 C 0.1159(3) 0.7039(3) 0.3668(3) 0.0409(15) Uani 0.689(8) 1 d PD A 1 H18 H 0.1512 0.6697 0.4020 0.049 Uiso 0.689(8) 1 calc PR A 1 C19 C 0.1163(2) 0.7908(3) 0.3784(3) 0.0634(16) Uani 0.689(8) 1 d PD A 1 H19A H 0.0818 0.8274 0.3446 0.076 Uiso 0.689(8) 1 calc PR A 1 H19B H 0.1510 0.8163 0.4206 0.076 Uiso 0.689(8) 1 calc PR A 1 C18A C 0.0971(6) 0.7311(6) 0.3520(7) 0.035(3) Uani 0.311(8) 1 d PD . 2 H18A H 0.0713 0.7850 0.3414 0.042 Uiso 0.311(8) 1 calc PR A 2 C19A C 0.1588(5) 0.7312(7) 0.4088(5) 0.062(3) Uani 0.311(8) 1 d PD A 2 H19C H 0.1860 0.6785 0.4210 0.075 Uiso 0.311(8) 1 calc PR A 2 H19D H 0.1751 0.7840 0.4366 0.075 Uiso 0.311(8) 1 calc PR A 2 C20A C 0.5222(5) 0.4533(10) 0.7252(5) 0.203(8) Uani 0.630(14) 1 d PD . 1 H20A H 0.5520 0.5070 0.7347 0.244 Uiso 0.630(14) 1 calc PR . 1 H20B H 0.5531 0.4005 0.7359 0.244 Uiso 0.630(14) 1 calc PR . 1 C21A C 0.4760(5) 0.4518(6) 0.6466(6) 0.144(5) Uani 0.630(14) 1 d PD . 1 H21C H 0.4423 0.5015 0.6386 0.173 Uiso 0.630(14) 1 calc PR . 1 H21D H 0.4488 0.3959 0.6375 0.173 Uiso 0.630(14) 1 calc PR . 1 C22A C 0.5126(6) 0.4590(11) 0.5902(7) 0.126(6) Uani 0.630(14) 1 d PD . 1 H22A H 0.5076 0.5195 0.5701 0.189 Uiso 0.630(14) 1 calc PR . 1 H22B H 0.4919 0.4169 0.5492 0.189 Uiso 0.630(14) 1 calc PR . 1 H22C H 0.5624 0.4453 0.6143 0.189 Uiso 0.630(14) 1 calc PR . 1 C20B C 0.4868(7) 0.4556(7) 0.7077(3) 0.097(5) Uani 0.370(14) 1 d PD . 2 H20C H 0.4557 0.4037 0.6898 0.117 Uiso 0.370(14) 1 calc PR . 2 H20D H 0.4584 0.5098 0.6898 0.117 Uiso 0.370(14) 1 calc PR . 2 C21B C 0.5419(5) 0.4526(6) 0.6750(5) 0.071(4) Uani 0.370(14) 1 d PD . 2 H21A H 0.5762 0.4057 0.6994 0.085 Uiso 0.370(14) 1 calc PR . 2 H21B H 0.5668 0.5102 0.6821 0.085 Uiso 0.370(14) 1 calc PR . 2 C22B C 0.5089(11) 0.433(2) 0.5933(7) 0.156(13) Uani 0.370(14) 1 d PD . 2 H22D H 0.4895 0.3729 0.5868 0.235 Uiso 0.370(14) 1 calc PR . 2 H22E H 0.5443 0.4379 0.5684 0.235 Uiso 0.370(14) 1 calc PR . 2 H22F H 0.4712 0.4759 0.5709 0.235 Uiso 0.370(14) 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0637(11) 0.0389(8) 0.0520(10) 0.0010(7) 0.0307(9) 0.0001(8) N1 0.0361(10) 0.0407(9) 0.0310(9) -0.0010(8) 0.0108(8) 0.0019(8) C1 0.0398(14) 0.0626(15) 0.0393(13) -0.0092(11) 0.0115(11) -0.0049(11) Li1 0.037(2) 0.0361(18) 0.0335(18) -0.0032(14) 0.0135(15) 0.0001(15) O2 0.0311(8) 0.0313(7) 0.0276(7) -0.0024(6) 0.0109(6) -0.0024(6) N2 0.0514(12) 0.0364(9) 0.0342(10) 0.0010(8) 0.0144(9) 0.0084(9) C2 0.0428(15) 0.100(2) 0.0434(14) -0.0194(14) 0.0158(12) -0.0125(15) Li2 0.037(2) 0.0437(19) 0.0314(18) 0.0017(15) 0.0132(16) 0.0030(15) O3 0.0413(9) 0.0348(8) 0.0305(8) -0.0077(6) 0.0108(7) -0.0063(6) N3 0.0377(11) 0.0489(10) 0.0338(10) -0.0029(8) 0.0156(8) -0.0073(9) C3 0.0426(16) 0.125(3) 0.0383(14) 0.0092(15) 0.0125(12) 0.0220(17) Li3 0.040(2) 0.0325(17) 0.0330(18) 0.0030(14) 0.0136(15) -0.0036(15) N4 0.0496(12) 0.0358(9) 0.0340(10) 0.0019(8) 0.0133(9) -0.0064(8) C4 0.0625(18) 0.0672(16) 0.0441(14) 0.0157(12) 0.0272(13) 0.0268(14) C5 0.0397(13) 0.0459(12) 0.0345(12) -0.0008(10) 0.0179(10) 0.0095(10) C6 0.108(3) 0.0406(13) 0.094(2) 0.0057(14) 0.067(2) 0.0046(15) C7 0.0715(18) 0.0391(12) 0.0575(16) -0.0008(11) 0.0269(14) -0.0093(12) C8 0.0654(17) 0.0527(14) 0.0389(13) 0.0115(11) 0.0159(12) 0.0001(12) C9 0.0462(14) 0.0444(12) 0.0318(11) -0.0015(9) 0.0142(10) -0.0159(10) C10 0.0441(13) 0.0486(12) 0.0296(11) -0.0018(9) 0.0162(10) -0.0111(10) C11 0.0430(14) 0.0722(16) 0.0546(15) -0.0036(13) 0.0225(12) -0.0126(13) C12 0.0555(15) 0.0608(14) 0.0359(13) -0.0047(11) 0.0254(12) 0.0020(12) C13 0.0641(16) 0.0424(12) 0.0351(12) -0.0058(10) 0.0180(12) 0.0071(11) C14 0.0592(17) 0.0559(14) 0.0516(15) 0.0064(12) 0.0219(13) 0.0236(13) C15 0.0719(18) 0.0380(12) 0.0565(15) -0.0082(11) 0.0224(13) 0.0000(12) C16 0.0377(12) 0.0288(10) 0.0318(11) -0.0027(8) 0.0169(10) -0.0027(9) C17 0.0408(13) 0.0476(12) 0.0290(11) -0.0055(9) 0.0103(10) -0.0098(10) C18 0.041(4) 0.047(3) 0.032(3) -0.004(2) 0.009(3) 0.000(3) C19 0.071(3) 0.062(3) 0.063(3) -0.029(2) 0.030(2) -0.029(3) C18A 0.028(6) 0.031(7) 0.039(6) 0.007(5) 0.002(4) 0.007(4) C19A 0.056(7) 0.066(6) 0.055(6) -0.012(5) 0.005(5) -0.010(5) C20A 0.081(8) 0.316(17) 0.19(2) 0.003(11) 0.008(9) 0.046(8) C21A 0.110(8) 0.119(7) 0.181(13) 0.018(8) 0.017(8) -0.031(5) C22A 0.075(7) 0.111(6) 0.208(15) -0.029(6) 0.067(8) -0.022(5) C20B 0.158(15) 0.048(5) 0.105(12) -0.027(6) 0.068(12) -0.028(7) C21B 0.076(7) 0.054(5) 0.072(8) -0.006(4) 0.010(5) 0.009(4) C22B 0.116(17) 0.23(3) 0.075(11) -0.050(12) -0.038(10) 0.063(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C5 1.401(3) . ? O1 C6 1.427(3) . ? N1 C5 1.351(3) . ? N1 C1 1.469(3) . ? N1 Li1 2.016(4) . ? N1 Li2 2.041(4) . ? C1 C2 1.506(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? Li1 O2 1.966(4) . ? Li1 N2 2.105(4) . ? Li1 N3 2.212(4) . ? O2 C16 1.323(2) . ? O2 Li2 1.963(4) . ? O2 Li3 1.969(3) . ? N2 C14 1.464(3) . ? N2 C15 1.469(3) . ? N2 C13 1.470(3) . ? C2 C3 1.526(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? Li2 O3 1.932(4) . ? Li2 C17 2.517(4) 2 ? Li2 C16 2.564(4) 2 ? Li2 Li3 3.020(5) 2 ? O3 C18A 1.346(8) . ? O3 C18 1.351(5) . ? O3 Li3 1.960(4) 2 ? O3 Li3 1.964(4) . ? N3 C11 1.469(3) . ? N3 C10 1.470(3) . ? N3 C12 1.491(3) . ? C3 C4 1.498(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? Li3 O3 1.960(4) 2 ? Li3 N4 2.122(4) . ? Li3 Li3 2.558(6) 2 ? Li3 C18A 2.730(12) 2 ? Li3 Li2 3.020(5) 2 ? N4 C8 1.470(3) . ? N4 C9 1.471(3) . ? N4 C7 1.475(3) . ? C4 C5 1.350(3) . ? C4 H4 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.532(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.501(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.334(3) . ? C16 Li2 2.564(4) 2 ? C16 H16 0.9500 . ? C17 Li2 2.517(4) 2 ? C17 H17A 0.9500 . ? C17 H17B 0.9500 . ? C18 C19 1.326(6) . ? C18 H18 0.9500 . ? C19 H19A 0.9500 . ? C19 H19B 0.9500 . ? C18A C19A 1.349(9) . ? C18A Li3 2.730(12) 2 ? C18A H18A 0.9500 . ? C19A H19C 0.9500 . ? C19A H19D 0.9500 . ? C20A C21A 1.466(8) . ? C20A C20A 1.497(9) 2_656 ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? C21A C22A 1.487(9) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C20B C21B 1.443(9) . ? C20B C20B 1.504(10) 2_656 ? C20B H20C 0.9900 . ? C20B H20D 0.9900 . ? C21B C22B 1.491(9) . ? C21B H21A 0.9900 . ? C21B H21B 0.9900 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 O1 C6 117.9(2) . . ? C5 N1 C1 111.05(18) . . ? C5 N1 Li1 112.08(16) . . ? C1 N1 Li1 117.47(16) . . ? C5 N1 Li2 107.69(16) . . ? C1 N1 Li2 127.14(17) . . ? Li1 N1 Li2 77.28(15) . . ? N1 C1 C2 113.93(19) . . ? N1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? O2 Li1 N1 101.56(16) . . ? O2 Li1 N2 115.34(17) . . ? N1 Li1 N2 125.23(18) . . ? O2 Li1 N3 110.28(16) . . ? N1 Li1 N3 119.37(17) . . ? N2 Li1 N3 84.90(13) . . ? C16 O2 Li2 131.23(15) . . ? C16 O2 Li1 112.86(15) . . ? Li2 O2 Li1 80.30(15) . . ? C16 O2 Li3 112.05(15) . . ? Li2 O2 Li3 86.33(15) . . ? Li1 O2 Li3 130.02(15) . . ? C14 N2 C15 109.01(18) . . ? C14 N2 C13 113.31(18) . . ? C15 N2 C13 108.72(18) . . ? C14 N2 Li1 100.89(17) . . ? C15 N2 Li1 122.75(17) . . ? C13 N2 Li1 102.06(15) . . ? C1 C2 C3 109.2(2) . . ? C1 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? C1 C2 H2B 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? O3 Li2 O2 93.75(15) . . ? O3 Li2 N1 129.14(19) . . ? O2 Li2 N1 100.81(16) . . ? O3 Li2 C17 94.85(14) . 2 ? O2 Li2 C17 123.72(17) . 2 ? N1 Li2 C17 115.31(16) . 2 ? O3 Li2 C16 96.56(14) . 2 ? O2 Li2 C16 93.35(15) . 2 ? N1 Li2 C16 130.33(17) . 2 ? C17 Li2 C16 30.41(8) 2 2 ? O3 Li2 Li3 39.43(10) . 2 ? O2 Li2 Li3 86.44(14) . 2 ? N1 Li2 Li3 167.56(18) . 2 ? C17 Li2 Li3 67.32(11) 2 2 ? C16 Li2 Li3 58.41(10) 2 2 ? C18A O3 Li2 132.4(4) . . ? C18 O3 Li2 108.3(3) . . ? C18A O3 Li3 109.9(6) . 2 ? C18 O3 Li3 122.3(3) . 2 ? Li2 O3 Li3 101.81(15) . 2 ? C18A O3 Li3 131.0(6) . . ? C18 O3 Li3 146.1(3) . . ? Li2 O3 Li3 87.34(15) . . ? Li3 O3 Li3 81.39(16) 2 . ? C11 N3 C10 110.60(18) . . ? C11 N3 C12 108.14(18) . . ? C10 N3 C12 109.70(17) . . ? C11 N3 Li1 123.74(17) . . ? C10 N3 Li1 100.23(15) . . ? C12 N3 Li1 103.69(15) . . ? C4 C3 C2 110.6(2) . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? O3 Li3 O3 97.42(16) 2 . ? O3 Li3 O2 112.63(16) 2 . ? O3 Li3 O2 92.56(15) . . ? O3 Li3 N4 123.42(18) 2 . ? O3 Li3 N4 117.68(17) . . ? O2 Li3 N4 108.71(16) . . ? O3 Li3 Li3 49.38(12) 2 2 ? O3 Li3 Li3 49.24(12) . 2 ? O2 Li3 Li3 100.38(11) . 2 ? N4 Li3 Li3 149.08(10) . 2 ? O3 Li3 C18A 27.6(3) 2 2 ? O3 Li3 C18A 109.7(3) . 2 ? O2 Li3 C18A 133.8(3) . 2 ? N4 Li3 C18A 96.2(3) . 2 ? Li3 Li3 C18A 69.6(3) 2 2 ? O3 Li3 Li2 38.76(10) 2 2 ? O3 Li3 Li2 100.23(14) . 2 ? O2 Li3 Li2 73.88(12) . 2 ? N4 Li3 Li2 141.52(17) . 2 ? Li3 Li3 Li2 56.94(13) 2 2 ? C18A Li3 Li2 62.9(2) 2 2 ? C8 N4 C9 111.86(18) . . ? C8 N4 C7 108.82(18) . . ? C9 N4 C7 107.96(18) . . ? C8 N4 Li3 122.82(17) . . ? C9 N4 Li3 104.22(15) . . ? C7 N4 Li3 99.87(16) . . ? C5 C4 C3 119.8(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 N1 129.1(2) . . ? C4 C5 O1 123.5(2) . . ? N1 C5 O1 107.34(18) . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 H7A 109.5 . . ? N4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 C10 114.01(17) . . ? N4 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? N4 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? N3 C10 C9 112.68(17) . . ? N3 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? N3 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 C13 113.41(17) . . ? N3 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N3 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? N2 C13 C12 112.26(19) . . ? N2 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? N2 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 C17 126.65(18) . . ? O2 C16 Li2 101.66(13) . 2 ? C17 C16 Li2 72.84(15) . 2 ? O2 C16 H16 116.7 . . ? C17 C16 H16 116.7 . . ? Li2 C16 H16 95.9 2 . ? C16 C17 Li2 76.75(14) . 2 ? C16 C17 H17A 120.0 . . ? Li2 C17 H17A 98.2 2 . ? C16 C17 H17B 120.0 . . ? Li2 C17 H17B 94.9 2 . ? H17A C17 H17B 120.0 . . ? C19 C18 O3 125.5(5) . . ? C19 C18 H18 117.2 . . ? O3 C18 H18 117.2 . . ? C18 C19 H19A 120.0 . . ? C18 C19 H19B 120.0 . . ? H19A C19 H19B 120.0 . . ? O3 C18A C19A 124.7(9) . . ? C19A C18A Li3 142.6(10) . 2 ? O3 C18A H18A 117.7 . . ? C19A C18A H18A 117.7 . . ? Li3 C18A H18A 86.5 2 . ? C18A C19A H19C 120.0 . . ? C18A C19A H19D 120.0 . . ? H19C C19A H19D 120.0 . . ? C21A C20A C20A 108.6(10) . 2_656 ? C21A C20A H20A 110.0 . . ? C20A C20A H20A 110.0 2_656 . ? C21A C20A H20B 110.0 . . ? C20A C20A H20B 110.0 2_656 . ? H20A C20A H20B 108.3 . . ? C20A C21A C22A 114.8(8) . . ? C20A C21A H21C 108.6 . . ? C22A C21A H21C 108.6 . . ? C20A C21A H21D 108.6 . . ? C22A C21A H21D 108.6 . . ? H21C C21A H21D 107.5 . . ? C21B C20B C20B 113.6(14) . 2_656 ? C21B C20B H20C 108.8 . . ? C20B C20B H20C 108.8 2_656 . ? C21B C20B H20D 108.8 . . ? C20B C20B H20D 108.8 2_656 . ? H20C C20B H20D 107.7 . . ? C20B C21B C22B 107.7(12) . . ? C20B C21B H21A 110.2 . . ? C22B C21B H21A 110.2 . . ? C20B C21B H21B 110.2 . . ? C22B C21B H21B 110.2 . . ? H21A C21B H21B 108.5 . . ? C21B C22B H22D 109.5 . . ? C21B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C21B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.236 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.037 data_cmp5 _database_code_depnum_ccdc_archive 'CCDC 764918' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H52 N6 Na2 O2' _chemical_formula_sum 'C24 H52 N6 Na2 O2' _chemical_formula_weight 502.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.320(2) _cell_length_b 19.468(4) _cell_length_c 15.943(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.89(3) _cell_angle_gamma 90.00 _cell_volume 3048.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27362 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5358 _reflns_number_gt 4150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II v. 1.0 (Bruker AXS 2004)' _computing_cell_refinement 'Bruker APEX II v. 1.0 (Bruker AXS 2004)' _computing_data_reduction 'Bruker APEX II v. 1.0 (Bruker AXS 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+3.9003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5358 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1976 _refine_ls_wR_factor_gt 0.1820 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na -0.14268(11) 0.30949(5) 0.14500(7) 0.0277(3) Uani 1 1 d . . . Na2 Na 0.03180(10) 0.18973(5) 0.13753(7) 0.0259(3) Uani 1 1 d . . . O1 O -0.2138(2) 0.15507(14) 0.07948(14) 0.0497(6) Uani 1 1 d . . . O2 O 0.1691(2) 0.28835(10) 0.20524(13) 0.0365(5) Uani 1 1 d . . . N1 N -0.1453(3) 0.20203(13) 0.21225(17) 0.0392(6) Uani 1 1 d . . . N2 N 0.0236(2) 0.30572(11) 0.07159(15) 0.0275(5) Uani 1 1 d . . . N3 N -0.3645(2) 0.36328(12) 0.07022(15) 0.0279(5) Uani 1 1 d . . . N4 N -0.1452(2) 0.41650(12) 0.22863(15) 0.0305(5) Uani 1 1 d . . . N5 N 0.1128(2) 0.07118(12) 0.19445(15) 0.0306(5) Uani 1 1 d . . . N6 N 0.1738(2) 0.14165(11) 0.04833(15) 0.0297(5) Uani 1 1 d . . . C1 C -0.1506(4) 0.20281(18) 0.3008(2) 0.0456(8) Uani 1 1 d . . . H1A H -0.0939 0.2411 0.3333 0.055 Uiso 1 1 calc R . . H1B H -0.1119 0.1594 0.3304 0.055 Uiso 1 1 calc R . . C2 C -0.2920(4) 0.21089(19) 0.3045(2) 0.0470(8) Uani 1 1 d . . . H2A H -0.3307 0.2544 0.2753 0.056 Uiso 1 1 calc R . . H2B H -0.2904 0.2134 0.3668 0.056 Uiso 1 1 calc R . . C3 C -0.3811(4) 0.15167(19) 0.2598(2) 0.0502(9) Uani 1 1 d . . . H3A H -0.4781 0.1650 0.2457 0.060 Uiso 1 1 calc R . . H3B H -0.3649 0.1118 0.3002 0.060 Uiso 1 1 calc R . . C4 C -0.3502(3) 0.13127(16) 0.1740(2) 0.0410(8) Uani 1 1 d . . . H4 H -0.4038 0.0983 0.1344 0.049 Uiso 1 1 calc R . . C5 C -0.2443(3) 0.16233(14) 0.15868(17) 0.0261(6) Uani 1 1 d . . . C6 C -0.3140(4) 0.1196(3) 0.0088(2) 0.0698(14) Uani 1 1 d . . . H6A H -0.3248 0.0724 0.0272 0.105 Uiso 1 1 calc R . . H6B H -0.2835 0.1186 -0.0436 0.105 Uiso 1 1 calc R . . H6C H -0.4014 0.1437 -0.0049 0.105 Uiso 1 1 calc R . . C7 C -0.0022(3) 0.33478(15) -0.01639(19) 0.0338(7) Uani 1 1 d . . . H7A H -0.0998 0.3291 -0.0497 0.041 Uiso 1 1 calc R . . H7B H 0.0514 0.3091 -0.0480 0.041 Uiso 1 1 calc R . . C8 C 0.0346(3) 0.41010(16) -0.0140(2) 0.0397(7) Uani 1 1 d . . . H8A H -0.0194 0.4362 0.0169 0.048 Uiso 1 1 calc R . . H8B H 0.0125 0.4280 -0.0749 0.048 Uiso 1 1 calc R . . C9 C 0.1856(3) 0.41983(16) 0.0335(2) 0.0411(8) Uani 1 1 d . . . H9A H 0.2389 0.4066 -0.0061 0.049 Uiso 1 1 calc R . . H9B H 0.2042 0.4688 0.0493 0.049 Uiso 1 1 calc R . . C10 C 0.2285(3) 0.37627(14) 0.1159(2) 0.0340(7) Uani 1 1 d . . . H10 H 0.3145 0.3833 0.1590 0.041 Uiso 1 1 calc R . . C11 C 0.1427(3) 0.32712(13) 0.12760(18) 0.0270(6) Uani 1 1 d . . . C12 C 0.2911(4) 0.30245(19) 0.2747(2) 0.0507(9) Uani 1 1 d . . . H12A H 0.3699 0.2939 0.2541 0.076 Uiso 1 1 calc R . . H12B H 0.2960 0.2726 0.3250 0.076 Uiso 1 1 calc R . . H12C H 0.2913 0.3506 0.2927 0.076 Uiso 1 1 calc R . . C15 C -0.1705(4) 0.4068(2) 0.3128(2) 0.0560(10) Uani 1 1 d . . . H15A H -0.0979 0.3785 0.3514 0.084 Uiso 1 1 calc R . . H15B H -0.2584 0.3838 0.3032 0.084 Uiso 1 1 calc R . . H15C H -0.1722 0.4516 0.3406 0.084 Uiso 1 1 calc R . . C16 C -0.0148(3) 0.45088(18) 0.2429(2) 0.0453(8) Uani 1 1 d . . . H16A H -0.0180 0.4964 0.2685 0.068 Uiso 1 1 calc R . . H16B H 0.0037 0.4559 0.1865 0.068 Uiso 1 1 calc R . . H16C H 0.0575 0.4235 0.2833 0.068 Uiso 1 1 calc R . . C17 C -0.2538(3) 0.45846(15) 0.1687(2) 0.0393(7) Uani 1 1 d . . . H17A H -0.2210 0.4770 0.1211 0.047 Uiso 1 1 calc R . . H17B H -0.2744 0.4978 0.2019 0.047 Uiso 1 1 calc R . . C18 C -0.3822(3) 0.41806(16) 0.1285(2) 0.0380(7) Uani 1 1 d . . . H18A H -0.4124 0.3977 0.1762 0.046 Uiso 1 1 calc R . . H18B H -0.4546 0.4496 0.0946 0.046 Uiso 1 1 calc R . . C19 C -0.4720(3) 0.31127(16) 0.0577(2) 0.0412(8) Uani 1 1 d . . . H19A H -0.5610 0.3326 0.0303 0.062 Uiso 1 1 calc R . . H19B H -0.4692 0.2920 0.1150 0.062 Uiso 1 1 calc R . . H19C H -0.4575 0.2746 0.0195 0.062 Uiso 1 1 calc R . . C20 C -0.3672(4) 0.38982(19) -0.0157(2) 0.0503(9) Uani 1 1 d . . . H20A H -0.3564 0.3518 -0.0532 0.075 Uiso 1 1 calc R . . H20B H -0.2927 0.4227 -0.0085 0.075 Uiso 1 1 calc R . . H20C H -0.4544 0.4128 -0.0432 0.075 Uiso 1 1 calc R . . C21 C 0.0050(3) 0.03506(18) 0.2180(3) 0.0491(9) Uani 1 1 d . . . H21A H 0.0372 -0.0107 0.2407 0.074 Uiso 1 1 calc R . . H21B H -0.0749 0.0305 0.1656 0.074 Uiso 1 1 calc R . . H21C H -0.0199 0.0611 0.2633 0.074 Uiso 1 1 calc R . . C22 C 0.2304(4) 0.0781(2) 0.2723(2) 0.0534(9) Uani 1 1 d . . . H22A H 0.2047 0.1038 0.3176 0.080 Uiso 1 1 calc R . . H22B H 0.3028 0.1027 0.2570 0.080 Uiso 1 1 calc R . . H22C H 0.2630 0.0324 0.2950 0.080 Uiso 1 1 calc R . . C23 C 0.1436(4) 0.03411(15) 0.1233(2) 0.0410(8) Uani 1 1 d . . . H23A H 0.0573 0.0224 0.0775 0.049 Uiso 1 1 calc R . . H23B H 0.1903 -0.0094 0.1469 0.049 Uiso 1 1 calc R . . C24 C 0.2321(4) 0.07466(15) 0.0817(2) 0.0422(8) Uani 1 1 d . . . H24A H 0.3224 0.0817 0.1258 0.051 Uiso 1 1 calc R . . H24B H 0.2457 0.0477 0.0324 0.051 Uiso 1 1 calc R . . C25 C 0.2795(3) 0.18760(15) 0.0385(2) 0.0341(7) Uani 1 1 d . . . H25A H 0.3160 0.1697 -0.0071 0.051 Uiso 1 1 calc R . . H25B H 0.3528 0.1907 0.0946 0.051 Uiso 1 1 calc R . . H25C H 0.2407 0.2333 0.0214 0.051 Uiso 1 1 calc R . . C26 C 0.0648(4) 0.13677(18) -0.0341(2) 0.0490(8) Uani 1 1 d . . . H26A H 0.0998 0.1165 -0.0791 0.074 Uiso 1 1 calc R . . H26B H 0.0290 0.1828 -0.0529 0.074 Uiso 1 1 calc R . . H26C H -0.0081 0.1078 -0.0261 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0281(6) 0.0213(5) 0.0396(6) 0.0036(4) 0.0192(5) 0.0053(4) Na2 0.0251(6) 0.0176(5) 0.0387(6) -0.0003(4) 0.0150(5) 0.0019(4) O1 0.0328(12) 0.0820(18) 0.0376(12) 0.0048(12) 0.0159(10) 0.0003(12) O2 0.0479(13) 0.0285(11) 0.0311(10) 0.0024(8) 0.0091(9) -0.0079(9) N1 0.0463(16) 0.0284(13) 0.0375(14) 0.0023(11) 0.0048(12) -0.0033(11) N2 0.0255(12) 0.0266(12) 0.0340(12) 0.0030(10) 0.0143(10) 0.0010(10) N3 0.0239(12) 0.0255(12) 0.0349(12) -0.0005(10) 0.0102(10) -0.0010(10) N4 0.0267(12) 0.0310(13) 0.0359(12) -0.0050(10) 0.0126(10) -0.0020(10) N5 0.0336(13) 0.0271(12) 0.0351(12) 0.0055(10) 0.0163(11) 0.0062(10) N6 0.0374(13) 0.0213(12) 0.0367(13) 0.0003(10) 0.0205(11) 0.0004(10) C1 0.052(2) 0.0432(19) 0.0417(18) 0.0007(15) 0.0137(16) -0.0010(16) C2 0.057(2) 0.050(2) 0.0383(17) -0.0010(15) 0.0216(16) -0.0125(17) C3 0.050(2) 0.050(2) 0.060(2) 0.0042(17) 0.0309(18) -0.0034(17) C4 0.0337(17) 0.0312(16) 0.063(2) 0.0072(15) 0.0215(15) 0.0009(13) C5 0.0293(14) 0.0229(13) 0.0284(13) -0.0010(11) 0.0124(11) 0.0000(11) C6 0.041(2) 0.135(4) 0.0303(17) -0.018(2) 0.0062(15) 0.016(2) C7 0.0328(16) 0.0323(15) 0.0381(16) 0.0051(12) 0.0136(13) 0.0026(13) C8 0.0461(19) 0.0311(16) 0.0454(17) 0.0059(13) 0.0193(15) 0.0025(14) C9 0.0453(19) 0.0265(15) 0.059(2) 0.0088(14) 0.0270(16) -0.0014(13) C10 0.0285(15) 0.0268(15) 0.0488(17) -0.0011(13) 0.0150(13) -0.0032(12) C11 0.0277(14) 0.0195(13) 0.0376(15) 0.0028(11) 0.0157(12) 0.0037(11) C12 0.058(2) 0.046(2) 0.0384(17) -0.0006(15) 0.0012(16) -0.0114(17) C15 0.065(2) 0.063(2) 0.0454(19) -0.0052(18) 0.0259(18) -0.013(2) C16 0.0358(18) 0.0448(19) 0.059(2) -0.0138(16) 0.0192(15) -0.0078(15) C17 0.0381(17) 0.0249(15) 0.0555(19) -0.0066(14) 0.0155(15) 0.0025(13) C18 0.0291(16) 0.0345(16) 0.0506(18) -0.0050(14) 0.0123(14) 0.0084(13) C19 0.0359(17) 0.0364(17) 0.0528(19) 0.0025(14) 0.0157(15) -0.0059(14) C20 0.059(2) 0.051(2) 0.0419(18) 0.0030(15) 0.0164(16) -0.0165(18) C21 0.0392(19) 0.0395(19) 0.074(2) 0.0201(17) 0.0255(17) 0.0053(15) C22 0.050(2) 0.066(2) 0.0432(19) 0.0042(17) 0.0137(16) -0.0072(18) C23 0.056(2) 0.0222(15) 0.0499(19) 0.0016(13) 0.0238(16) 0.0046(14) C24 0.060(2) 0.0260(15) 0.0561(19) 0.0033(14) 0.0399(17) 0.0125(14) C25 0.0355(16) 0.0317(16) 0.0399(16) 0.0034(12) 0.0187(13) 0.0001(13) C26 0.052(2) 0.0438(19) 0.052(2) -0.0080(16) 0.0180(17) -0.0105(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 N1 2.355(3) . ? Na1 N2 2.357(2) . ? Na1 N3 2.466(3) . ? Na1 N4 2.478(3) . ? Na2 O2 2.433(2) . ? Na2 N1 2.480(3) . ? Na2 N2 2.481(2) . ? Na2 O1 2.509(3) . ? Na2 N6 2.515(2) . ? Na2 N5 2.526(2) . ? O1 C5 1.399(3) . ? O1 C6 1.449(5) . ? O2 C11 1.403(3) . ? O2 C12 1.425(4) . ? N1 C5 1.355(4) . ? N1 C1 1.430(4) . ? N2 C11 1.344(4) . ? N2 C7 1.459(4) . ? N3 C20 1.456(4) . ? N3 C18 1.462(4) . ? N3 C19 1.470(4) . ? N4 C16 1.456(4) . ? N4 C15 1.456(4) . ? N4 C17 1.476(4) . ? N5 C22 1.451(4) . ? N5 C21 1.459(4) . ? N5 C23 1.459(4) . ? N6 C26 1.447(4) . ? N6 C25 1.456(4) . ? N6 C24 1.466(4) . ? C1 C2 1.487(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.511(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.548(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.336(4) . ? C4 H4 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.512(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.521(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.512(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.355(4) . ? C10 H10 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.504(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.506(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Na1 N2 108.08(9) . . ? N1 Na1 N3 117.32(9) . . ? N2 Na1 N3 118.84(9) . . ? N1 Na1 N4 119.90(10) . . ? N2 Na1 N4 115.02(9) . . ? N3 Na1 N4 75.02(8) . . ? O2 Na2 N1 97.20(9) . . ? O2 Na2 N2 53.79(8) . . ? N1 Na2 N2 100.45(8) . . ? O2 Na2 O1 139.52(9) . . ? N1 Na2 O1 52.65(8) . . ? N2 Na2 O1 100.91(9) . . ? O2 Na2 N6 100.56(8) . . ? N1 Na2 N6 161.91(9) . . ? N2 Na2 N6 92.81(8) . . ? O1 Na2 N6 112.92(9) . . ? O2 Na2 N5 118.56(9) . . ? N1 Na2 N5 97.30(9) . . ? N2 Na2 N5 161.44(8) . . ? O1 Na2 N5 94.14(9) . . ? N6 Na2 N5 71.16(8) . . ? C5 O1 C6 116.4(2) . . ? C5 O1 Na2 96.98(17) . . ? C6 O1 Na2 144.5(2) . . ? C11 O2 C12 117.9(2) . . ? C11 O2 Na2 95.97(15) . . ? C12 O2 Na2 138.76(19) . . ? C5 N1 C1 112.2(3) . . ? C5 N1 Na1 109.36(18) . . ? C1 N1 Na1 116.7(2) . . ? C5 N1 Na2 99.58(18) . . ? C1 N1 Na2 137.1(2) . . ? Na1 N1 Na2 75.76(8) . . ? C11 N2 C7 112.2(2) . . ? C11 N2 Na1 108.48(17) . . ? C7 N2 Na1 121.31(18) . . ? C11 N2 Na2 95.47(16) . . ? C7 N2 Na2 137.10(18) . . ? Na1 N2 Na2 75.71(7) . . ? C20 N3 C18 111.6(3) . . ? C20 N3 C19 108.7(2) . . ? C18 N3 C19 110.6(2) . . ? C20 N3 Na1 110.7(2) . . ? C18 N3 Na1 106.33(17) . . ? C19 N3 Na1 108.84(18) . . ? C16 N4 C15 109.5(3) . . ? C16 N4 C17 109.2(2) . . ? C15 N4 C17 110.6(3) . . ? C16 N4 Na1 107.98(18) . . ? C15 N4 Na1 114.9(2) . . ? C17 N4 Na1 104.40(17) . . ? C22 N5 C21 109.1(3) . . ? C22 N5 C23 112.7(3) . . ? C21 N5 C23 109.1(3) . . ? C22 N5 Na2 108.7(2) . . ? C21 N5 Na2 109.76(18) . . ? C23 N5 Na2 107.45(17) . . ? C26 N6 C25 110.0(2) . . ? C26 N6 C24 112.9(3) . . ? C25 N6 C24 110.4(2) . . ? C26 N6 Na2 96.46(18) . . ? C25 N6 Na2 114.71(17) . . ? C24 N6 Na2 111.78(16) . . ? N1 C1 C2 112.1(3) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 C3 111.3(3) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 110.6(3) . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 116.6(3) . . ? C5 C4 H4 121.7 . . ? C3 C4 H4 121.7 . . ? C4 C5 N1 130.1(3) . . ? C4 C5 O1 122.9(3) . . ? N1 C5 O1 107.0(2) . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 112.4(2) . . ? N2 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N2 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 110.1(3) . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C8 110.1(2) . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 119.1(3) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? N2 C11 C10 129.1(3) . . ? N2 C11 O2 108.1(2) . . ? C10 C11 O2 122.9(3) . . ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C15 H15A 109.5 . . ? N4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 H16A 109.5 . . ? N4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 C18 112.4(2) . . ? N4 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? N4 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? N3 C18 C17 112.8(2) . . ? N3 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? N3 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 H21A 109.5 . . ? N5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 H22A 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N5 C23 C24 112.9(3) . . ? N5 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? N5 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N6 C24 C23 112.9(2) . . ? N6 C24 H24A 109.0 . . ? C23 C24 H24A 109.0 . . ? N6 C24 H24B 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? N6 C25 H25A 109.5 . . ? N6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N6 C26 H26A 109.5 . . ? N6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.274 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.065 data_cmp6 _database_code_depnum_ccdc_archive 'CCDC 764919' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H116 K4 Li4 N12 O8' _chemical_formula_sum 'C52 H116 K4 Li4 N12 O8' _chemical_formula_weight 1221.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 19.661(4) _cell_length_b 21.434(4) _cell_length_c 17.180(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7240(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cubic _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 0.297 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9541 _exptl_absorpt_correction_T_max 0.9708 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55794 _diffrn_reflns_av_R_equivalents 0.0946 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6384 _reflns_number_gt 3759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-seed / POV-Ray' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1138P)^2^+10.7940P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6384 _refine_ls_number_parameters 375 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1375 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.2471 _refine_ls_wR_factor_gt 0.2073 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.16499(5) 0.19701(6) 0.17386(6) 0.0598(4) Uani 1 1 d . . . K2 K 0.0000 0.03465(6) 0.2500 0.0713(6) Uani 1 2 d S . . K3 K 0.0000 0.36067(6) 0.2500 0.0506(4) Uani 1 2 d S . . O1 O 0.1594(2) 0.05484(19) 0.2095(2) 0.0834(13) Uani 1 1 d . . . O2 O 0.1340(2) 0.34447(19) 0.1590(2) 0.0828(13) Uani 1 1 d . . . O3 O 0.03102(14) 0.14793(12) 0.17415(14) 0.0358(6) Uani 1 1 d . . . O4 O 0.06831(13) 0.24595(11) 0.28051(14) 0.0341(6) Uani 1 1 d . . . N1 N 0.1354(3) 0.1049(2) 0.3195(2) 0.0729(14) Uani 1 1 d . . . N2 N 0.0534(2) 0.29210(18) 0.0940(2) 0.0563(11) Uani 1 1 d . . . N3 N 0.2649(2) 0.1781(2) 0.0481(3) 0.0756(14) Uani 1 1 d . . . N4 N 0.3078(2) 0.2164(2) 0.2067(3) 0.0807(14) Uani 1 1 d . . . N5 N 0.0049(3) -0.07994(18) 0.3399(2) 0.0625(12) Uani 1 1 d . . . N6 N -0.0273(3) 0.4758(2) 0.1686(3) 0.0782(15) Uani 1 1 d . . . C1 C 0.1516(5) 0.1145(4) 0.4011(4) 0.156(5) Uani 1 1 d . . . H1A H 0.1724 0.1565 0.4043 0.187 Uiso 1 1 calc R . . H1B H 0.1073 0.1175 0.4284 0.187 Uiso 1 1 calc R . . C2 C 0.1881(5) 0.0796(5) 0.4421(4) 0.147(4) Uani 1 1 d . . . H2A H 0.1572 0.0592 0.4799 0.177 Uiso 1 1 calc R . . H2B H 0.2182 0.1073 0.4727 0.177 Uiso 1 1 calc R . . C3 C 0.2316(3) 0.0302(3) 0.4105(3) 0.090(2) Uani 1 1 d D . . H3A H 0.2220 -0.0093 0.4382 0.108 Uiso 1 1 calc R . . H3B H 0.2798 0.0411 0.4196 0.108 Uiso 1 1 calc R . . C4 C 0.2205(3) 0.0208(2) 0.3260(3) 0.0710(16) Uani 1 1 d D . . H4 H 0.2446 -0.0104 0.2981 0.085 Uiso 1 1 calc R . . C5 C 0.1724(2) 0.0603(2) 0.2876(3) 0.0602(13) Uani 1 1 d DU . . C6 C 0.1969(3) 0.0109(3) 0.1648(4) 0.088(2) Uani 1 1 d . . . H6A H 0.2454 0.0208 0.1676 0.132 Uiso 1 1 calc R . . H6B H 0.1818 0.0126 0.1104 0.132 Uiso 1 1 calc R . . H6C H 0.1891 -0.0312 0.1854 0.132 Uiso 1 1 calc R . . C7 C 0.0142(3) 0.2843(3) 0.0227(3) 0.0766(17) Uani 1 1 d . . . H7A H -0.0124 0.2452 0.0267 0.092 Uiso 1 1 calc R . . H7B H -0.0186 0.3192 0.0185 0.092 Uiso 1 1 calc R . . C8 C 0.0537(4) 0.2822(4) -0.0472(3) 0.101(2) Uani 1 1 d . . . H8A H 0.0226 0.2799 -0.0924 0.121 Uiso 1 1 calc R . . H8B H 0.0817 0.2438 -0.0469 0.121 Uiso 1 1 calc R . . C9 C 0.1013(5) 0.3398(3) -0.0570(4) 0.107(3) Uani 1 1 d . . . H9A H 0.1395 0.3291 -0.0921 0.128 Uiso 1 1 calc R . . H9B H 0.0756 0.3747 -0.0806 0.128 Uiso 1 1 calc R . . C10 C 0.1283(4) 0.3592(3) 0.0201(3) 0.085(2) Uani 1 1 d . . . H10 H 0.1621 0.3908 0.0232 0.102 Uiso 1 1 calc R . . C11 C 0.1053(3) 0.3323(2) 0.0853(3) 0.0578(13) Uani 1 1 d . . . C12 C 0.1910(3) 0.3849(3) 0.1625(4) 0.090(2) Uani 1 1 d . . . H12A H 0.2290 0.3663 0.1338 0.135 Uiso 1 1 calc R . . H12B H 0.2042 0.3912 0.2169 0.135 Uiso 1 1 calc R . . H12C H 0.1792 0.4252 0.1390 0.135 Uiso 1 1 calc R . . C13 C 0.0415(3) 0.1186(2) 0.1020(2) 0.0518(12) Uani 1 1 d . . . H13A H 0.0707 0.0820 0.1092 0.078 Uiso 1 1 calc R . . H13B H 0.0636 0.1479 0.0662 0.078 Uiso 1 1 calc R . . H13C H -0.0023 0.1055 0.0804 0.078 Uiso 1 1 calc R . . C14 C 0.1181(2) 0.2759(2) 0.3242(3) 0.0499(11) Uani 1 1 d . . . H14A H 0.0965 0.3016 0.3643 0.075 Uiso 1 1 calc R . . H14B H 0.1457 0.3024 0.2901 0.075 Uiso 1 1 calc R . . H14C H 0.1474 0.2446 0.3491 0.075 Uiso 1 1 calc R . . C15 C 0.3357(4) 0.1791(5) 0.0741(5) 0.130(3) Uani 1 1 d U . . H15A H 0.3653 0.1886 0.0290 0.156 Uiso 1 1 calc R . . H15B H 0.3481 0.1370 0.0933 0.156 Uiso 1 1 calc R . . C16 C 0.3496(3) 0.2264(5) 0.1380(5) 0.115(3) Uani 1 1 d . . . H16A H 0.3981 0.2241 0.1530 0.138 Uiso 1 1 calc R . . H16B H 0.3409 0.2689 0.1176 0.138 Uiso 1 1 calc R . . C17 C 0.2537(6) 0.1308(5) -0.0059(5) 0.176(5) Uani 1 1 d . . . H17A H 0.2092 0.1367 -0.0305 0.264 Uiso 1 1 calc R . . H17B H 0.2548 0.0903 0.0205 0.264 Uiso 1 1 calc R . . H17C H 0.2894 0.1320 -0.0458 0.264 Uiso 1 1 calc R . . C18 C 0.2468(5) 0.2378(4) 0.0133(5) 0.134(3) Uani 1 1 d . . . H18A H 0.2783 0.2472 -0.0294 0.201 Uiso 1 1 calc R . . H18B H 0.2498 0.2707 0.0528 0.201 Uiso 1 1 calc R . . H18C H 0.2003 0.2358 -0.0069 0.201 Uiso 1 1 calc R . . C19 C 0.3239(4) 0.2646(4) 0.2649(5) 0.113(3) Uani 1 1 d . . . H19A H 0.2966 0.2576 0.3118 0.169 Uiso 1 1 calc R . . H19B H 0.3136 0.3059 0.2434 0.169 Uiso 1 1 calc R . . H19C H 0.3724 0.2624 0.2782 0.169 Uiso 1 1 calc R . . C20 C 0.3178(5) 0.1549(3) 0.2394(4) 0.113(3) Uani 1 1 d . . . H20A H 0.3072 0.1232 0.2000 0.169 Uiso 1 1 calc R . . H20B H 0.2878 0.1494 0.2844 0.169 Uiso 1 1 calc R . . H20C H 0.3653 0.1503 0.2559 0.169 Uiso 1 1 calc R . . C21 C 0.0096(5) -0.1307(3) 0.2890(3) 0.123(3) Uani 1 1 d D . . H21A H 0.0580 -0.1437 0.2898 0.148 Uiso 1 1 calc R . . H21B H -0.0163 -0.1650 0.3138 0.148 Uiso 1 1 calc R . . C22 C -0.0513(4) -0.0923(4) 0.3932(4) 0.118(3) Uani 1 1 d . . . H22A H -0.0929 -0.1000 0.3633 0.176 Uiso 1 1 calc R . . H22B H -0.0580 -0.0562 0.4273 0.176 Uiso 1 1 calc R . . H22C H -0.0407 -0.1291 0.4249 0.176 Uiso 1 1 calc R . . C23 C 0.0659(5) -0.0761(5) 0.3841(6) 0.158(4) Uani 1 1 d . . . H23A H 0.0706 -0.1136 0.4163 0.237 Uiso 1 1 calc R . . H23B H 0.0643 -0.0392 0.4177 0.237 Uiso 1 1 calc R . . H23C H 0.1048 -0.0729 0.3487 0.237 Uiso 1 1 calc R . . C24 C -0.0220(4) 0.5284(3) 0.2175(4) 0.102(3) Uani 1 1 d . . . H24A H -0.0683 0.5375 0.2372 0.123 Uiso 1 1 calc R . . H24B H -0.0087 0.5641 0.1842 0.123 Uiso 1 1 calc R . . C25 C -0.0849(7) 0.4697(4) 0.1238(8) 0.208(7) Uani 1 1 d . . . H25A H -0.1252 0.4720 0.1572 0.312 Uiso 1 1 calc R . . H25B H -0.0840 0.4294 0.0969 0.312 Uiso 1 1 calc R . . H25C H -0.0865 0.5035 0.0853 0.312 Uiso 1 1 calc R . . C26 C 0.0293(6) 0.4825(5) 0.1127(5) 0.180(5) Uani 1 1 d . . . H26A H 0.0329 0.4444 0.0813 0.270 Uiso 1 1 calc R . . H26B H 0.0719 0.4892 0.1411 0.270 Uiso 1 1 calc R . . H26C H 0.0205 0.5182 0.0785 0.270 Uiso 1 1 calc R . . Li1 Li 0.0602(4) 0.1559(3) 0.2834(4) 0.0385(16) Uani 1 1 d . . . Li2 Li 0.0227(3) 0.2390(3) 0.1792(4) 0.0366(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0405(6) 0.0847(8) 0.0540(7) -0.0128(6) 0.0093(5) -0.0054(5) K2 0.1446(17) 0.0284(7) 0.0409(8) 0.000 0.0072(9) 0.000 K3 0.0581(9) 0.0329(7) 0.0609(9) 0.000 -0.0142(7) 0.000 O1 0.088(3) 0.097(3) 0.065(2) -0.035(2) -0.014(2) 0.056(2) O2 0.085(3) 0.096(3) 0.068(2) 0.000(2) -0.002(2) -0.056(2) O3 0.0475(17) 0.0329(14) 0.0270(14) -0.0036(12) 0.0021(12) -0.0007(12) O4 0.0325(15) 0.0373(15) 0.0324(14) -0.0040(12) -0.0055(12) -0.0014(12) N1 0.096(3) 0.069(3) 0.054(3) -0.019(2) -0.023(2) 0.049(3) N2 0.067(3) 0.063(2) 0.039(2) 0.0082(19) -0.0035(19) -0.029(2) N3 0.068(3) 0.082(3) 0.077(3) -0.001(3) 0.032(3) 0.003(3) N4 0.056(3) 0.097(4) 0.090(4) 0.005(3) -0.010(3) -0.020(3) N5 0.106(4) 0.043(2) 0.039(2) 0.0069(18) -0.004(2) -0.005(2) N6 0.117(4) 0.052(3) 0.066(3) -0.002(2) -0.028(3) 0.027(3) C1 0.253(11) 0.144(7) 0.070(4) -0.045(5) -0.078(6) 0.145(8) C2 0.147(7) 0.233(10) 0.062(4) -0.021(5) -0.024(5) 0.121(8) C3 0.091(5) 0.076(4) 0.104(5) 0.008(4) -0.037(4) 0.024(3) C4 0.063(3) 0.050(3) 0.100(4) -0.014(3) -0.024(3) 0.019(3) C5 0.058(3) 0.054(3) 0.068(3) -0.008(3) -0.015(3) 0.016(2) C6 0.075(4) 0.090(4) 0.101(5) -0.041(4) 0.004(4) 0.033(3) C7 0.105(5) 0.081(4) 0.044(3) 0.012(3) -0.012(3) -0.024(3) C8 0.121(6) 0.134(6) 0.047(3) -0.001(4) 0.004(4) -0.031(5) C9 0.168(8) 0.090(5) 0.062(4) 0.026(4) 0.016(4) -0.031(5) C10 0.117(5) 0.060(3) 0.077(4) 0.003(3) 0.037(4) -0.031(3) C11 0.068(3) 0.051(3) 0.054(3) 0.001(2) 0.011(3) -0.015(3) C12 0.074(4) 0.080(4) 0.115(5) -0.016(4) 0.004(4) -0.039(3) C13 0.075(3) 0.048(3) 0.033(2) -0.007(2) 0.006(2) 0.001(2) C14 0.043(3) 0.057(3) 0.050(3) -0.010(2) -0.009(2) 0.003(2) C15 0.090(5) 0.169(7) 0.132(6) -0.001(5) 0.049(5) 0.016(5) C16 0.056(4) 0.177(8) 0.111(6) 0.003(6) 0.013(4) -0.027(5) C17 0.271(14) 0.143(8) 0.114(6) -0.054(6) 0.093(8) -0.065(8) C18 0.170(9) 0.124(7) 0.108(6) 0.019(5) 0.036(6) 0.023(6) C19 0.096(5) 0.119(6) 0.124(6) 0.000(5) -0.045(5) -0.029(4) C20 0.148(7) 0.094(5) 0.097(5) 0.006(4) -0.037(5) -0.015(5) C21 0.258(11) 0.054(3) 0.057(3) 0.008(3) -0.017(5) 0.035(5) C22 0.146(7) 0.120(6) 0.087(5) 0.039(4) 0.027(5) 0.026(5) C23 0.144(8) 0.180(9) 0.149(8) 0.076(7) -0.059(7) -0.083(7) C24 0.191(8) 0.047(3) 0.069(4) 0.008(3) -0.013(4) 0.016(4) C25 0.252(13) 0.115(7) 0.258(13) 0.059(8) -0.181(12) -0.016(8) C26 0.263(14) 0.182(10) 0.095(6) 0.000(6) 0.034(8) 0.092(10) Li1 0.049(4) 0.030(3) 0.037(4) -0.002(3) 0.002(3) 0.007(3) Li2 0.039(4) 0.036(3) 0.034(4) -0.001(3) 0.000(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O3 2.836(3) . ? K1 O4 2.841(3) . ? K1 N4 2.894(5) . ? K1 N3 2.948(4) . ? K1 O1 3.110(4) . ? K1 O2 3.229(5) . ? K1 N1 3.240(5) . ? K1 N2 3.295(4) . ? K2 O3 2.822(3) . ? K2 O3 2.822(3) 4 ? K2 N5 2.903(4) 4 ? K2 N5 2.903(4) . ? K2 Li1 2.913(7) 4 ? K2 C13 3.220(5) 4 ? K2 O1 3.239(4) . ? K2 O1 3.239(4) 4 ? K2 N1 3.283(5) . ? K2 N1 3.283(5) 4 ? K2 C5 3.494(5) 4 ? K2 K1 4.9340(16) 4 ? K3 O4 2.850(3) 4 ? K3 O4 2.850(3) . ? K3 N6 2.887(4) . ? K3 N6 2.887(4) 4 ? K3 Li2 2.913(7) 4 ? K3 O2 3.083(4) 4 ? K3 O2 3.083(4) . ? K3 C14 3.214(5) 4 ? K3 N2 3.231(4) . ? K3 N2 3.231(4) 4 ? K3 K1 4.9538(16) 4 ? O1 C5 1.370(6) . ? O1 C6 1.422(6) . ? O2 C11 1.411(6) . ? O2 C12 1.418(6) . ? O3 C13 1.405(5) . ? O3 Li1 1.944(8) 4 ? O3 Li2 1.960(7) . ? O3 Li1 1.970(7) . ? O4 C14 1.391(5) . ? O4 Li2 1.925(7) 4 ? O4 Li1 1.937(7) . ? O4 Li2 1.964(7) . ? N1 C5 1.318(6) . ? N1 C1 1.452(7) . ? N1 Li1 1.941(8) . ? N2 C11 1.344(6) . ? N2 C7 1.457(6) . ? N2 Li2 1.949(7) . ? N3 C17 1.392(9) . ? N3 C18 1.457(9) . ? N3 C15 1.463(9) . ? N4 C20 1.446(8) . ? N4 C16 1.454(8) . ? N4 C19 1.473(8) . ? N5 C21 1.399(7) . ? N5 C23 1.422(9) . ? N5 C22 1.459(8) . ? N6 C25 1.376(10) . ? N6 C24 1.409(7) . ? N6 C26 1.477(11) . ? C1 C2 1.254(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.466(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.481(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.431(4) . ? C4 H4 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.431(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.559(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.487(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.338(7) . ? C10 H10 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.520(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C21 1.393(8) 4 ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C24 1.414(13) 4 ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? Li1 O3 1.944(8) 4 ? Li1 Li2 2.499(9) 4 ? Li1 Li1 2.630(14) 4 ? Li2 O4 1.925(7) 4 ? Li2 Li1 2.499(9) 4 ? Li2 Li2 2.592(13) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 K1 O4 60.95(7) . . ? O3 K1 N4 162.54(13) . . ? O4 K1 N4 118.08(13) . . ? O3 K1 N3 124.67(12) . . ? O4 K1 N3 165.76(12) . . ? N4 K1 N3 61.06(15) . . ? O3 K1 O1 66.64(9) . . ? O4 K1 O1 102.19(9) . . ? N4 K1 O1 97.84(13) . . ? N3 K1 O1 91.89(12) . . ? O3 K1 O2 100.83(9) . . ? O4 K1 O2 64.10(9) . . ? N4 K1 O2 93.33(13) . . ? N3 K1 O2 101.68(12) . . ? O1 K1 O2 165.46(11) . . ? O3 K1 N1 66.79(10) . . ? O4 K1 N1 66.86(9) . . ? N4 K1 N1 96.38(14) . . ? N3 K1 N1 126.99(13) . . ? O1 K1 N1 40.92(10) . . ? O2 K1 N1 128.60(10) . . ? O3 K1 N2 67.14(9) . . ? O4 K1 N2 66.06(9) . . ? N4 K1 N2 129.71(13) . . ? N3 K1 N2 102.93(13) . . ? O1 K1 N2 131.65(10) . . ? O2 K1 N2 40.16(9) . . ? N1 K1 N2 125.39(11) . . ? O3 K2 O3 61.30(10) . 4 ? O3 K2 N5 119.29(9) . 4 ? O3 K2 N5 165.11(11) 4 4 ? O3 K2 N5 165.11(11) . . ? O3 K2 N5 119.29(9) 4 . ? N5 K2 N5 64.44(16) 4 . ? O3 K2 Li1 39.59(14) . 4 ? O3 K2 Li1 40.13(14) 4 4 ? N5 K2 Li1 129.55(16) 4 4 ? N5 K2 Li1 150.80(16) . 4 ? O3 K2 C13 86.47(10) . 4 ? O3 K2 C13 25.82(9) 4 4 ? N5 K2 C13 152.21(12) 4 4 ? N5 K2 C13 93.50(11) . 4 ? Li1 K2 C13 63.49(15) 4 4 ? O3 K2 O1 64.97(9) . . ? O3 K2 O1 101.15(9) 4 . ? N5 K2 O1 91.75(12) 4 . ? N5 K2 O1 101.27(13) . . ? Li1 K2 O1 103.40(15) 4 . ? C13 K2 O1 109.89(11) 4 . ? O3 K2 O1 101.15(9) . 4 ? O3 K2 O1 64.97(9) 4 4 ? N5 K2 O1 101.27(13) 4 4 ? N5 K2 O1 91.75(12) . 4 ? Li1 K2 O1 61.96(15) 4 4 ? C13 K2 O1 60.69(12) 4 4 ? O1 K2 O1 164.65(14) . 4 ? O3 K2 N1 66.31(9) . . ? O3 K2 N1 67.24(9) 4 . ? N5 K2 N1 127.44(12) 4 . ? N5 K2 N1 99.66(12) . . ? Li1 K2 N1 89.55(15) 4 . ? C13 K2 N1 70.28(12) 4 . ? O1 K2 N1 39.84(10) . . ? O1 K2 N1 130.20(10) 4 . ? O3 K2 N1 67.24(9) . 4 ? O3 K2 N1 66.31(9) 4 4 ? N5 K2 N1 99.66(12) 4 4 ? N5 K2 N1 127.44(12) . 4 ? Li1 K2 N1 35.89(15) 4 4 ? C13 K2 N1 79.92(12) 4 4 ? O1 K2 N1 130.20(10) . 4 ? O1 K2 N1 39.84(10) 4 4 ? N1 K2 N1 125.43(14) . 4 ? O3 K2 C5 89.35(10) . 4 ? O3 K2 C5 74.93(10) 4 4 ? N5 K2 C5 90.18(13) 4 4 ? N5 K2 C5 105.28(13) . 4 ? Li1 K2 C5 55.16(15) 4 4 ? C13 K2 C5 79.15(13) 4 4 ? O1 K2 C5 151.38(11) . 4 ? O1 K2 C5 23.09(11) 4 4 ? N1 K2 C5 141.41(11) . 4 ? N1 K2 C5 22.15(10) 4 4 ? O3 K2 K1 69.98(6) . 4 ? O3 K2 K1 29.39(6) 4 4 ? N5 K2 K1 135.74(10) 4 4 ? N5 K2 K1 118.51(9) . 4 ? Li1 K2 K1 32.40(13) 4 4 ? C13 K2 K1 39.62(9) 4 4 ? O1 K2 K1 126.79(8) . 4 ? O1 K2 K1 38.07(7) 4 4 ? N1 K2 K1 96.52(7) . 4 ? N1 K2 K1 40.52(8) 4 4 ? C5 K2 K1 45.58(8) 4 4 ? O4 K3 O4 60.77(10) 4 . ? O4 K3 N6 124.12(11) 4 . ? O4 K3 N6 156.08(13) . . ? O4 K3 N6 156.09(12) 4 4 ? O4 K3 N6 124.12(11) . 4 ? N6 K3 N6 62.48(19) . 4 ? O4 K3 Li2 39.82(14) 4 4 ? O4 K3 Li2 39.01(14) . 4 ? N6 K3 Li2 159.95(17) . 4 ? N6 K3 Li2 126.30(16) 4 4 ? O4 K3 O2 66.01(9) 4 4 ? O4 K3 O2 102.26(9) . 4 ? N6 K3 O2 100.54(14) . 4 ? N6 K3 O2 90.55(14) 4 4 ? Li2 K3 O2 63.66(15) 4 4 ? O4 K3 O2 102.26(9) 4 . ? O4 K3 O2 66.01(9) . . ? N6 K3 O2 90.55(14) . . ? N6 K3 O2 100.54(14) 4 . ? Li2 K3 O2 104.01(15) 4 . ? O2 K3 O2 167.07(16) 4 . ? O4 K3 C14 25.64(9) 4 4 ? O4 K3 C14 85.73(10) . 4 ? N6 K3 C14 99.04(13) . 4 ? N6 K3 C14 144.11(15) 4 4 ? Li2 K3 C14 63.14(15) 4 4 ? O2 K3 C14 61.30(12) 4 4 ? O2 K3 C14 110.66(11) . 4 ? O4 K3 N2 66.93(8) 4 . ? O4 K3 N2 66.87(9) . . ? N6 K3 N2 92.73(12) . . ? N6 K3 N2 136.90(13) 4 . ? Li2 K3 N2 89.36(15) 4 . ? O2 K3 N2 130.29(11) 4 . ? O2 K3 N2 41.49(9) . . ? C14 K3 N2 69.40(11) 4 . ? O4 K3 N2 66.87(9) 4 4 ? O4 K3 N2 66.93(8) . 4 ? N6 K3 N2 136.90(13) . 4 ? N6 K3 N2 92.73(12) 4 4 ? Li2 K3 N2 36.53(14) 4 4 ? O2 K3 N2 41.49(9) 4 4 ? O2 K3 N2 130.29(11) . 4 ? C14 K3 N2 80.63(11) 4 4 ? N2 K3 N2 125.89(14) . 4 ? O4 K3 K1 29.44(5) 4 4 ? O4 K3 K1 69.46(6) . 4 ? N6 K3 K1 127.71(12) . 4 ? N6 K3 K1 126.82(11) 4 4 ? Li2 K3 K1 32.33(13) 4 4 ? O2 K3 K1 39.36(8) 4 4 ? O2 K3 K1 127.86(8) . 4 ? C14 K3 K1 39.72(8) 4 4 ? N2 K3 K1 96.28(7) . 4 ? N2 K3 K1 41.09(7) 4 4 ? C5 O1 C6 119.3(4) . . ? C5 O1 K1 95.8(3) . . ? C6 O1 K1 121.7(4) . . ? C5 O1 K2 88.9(3) . . ? C6 O1 K2 121.9(4) . . ? K1 O1 K2 101.96(9) . . ? C11 O2 C12 117.8(4) . . ? C11 O2 K3 97.7(3) . . ? C12 O2 K3 125.8(4) . . ? C11 O2 K1 88.0(3) . . ? C12 O2 K1 116.5(4) . . ? K3 O2 K1 103.38(10) . . ? C13 O3 Li1 120.4(3) . 4 ? C13 O3 Li2 119.8(3) . . ? Li1 O3 Li2 79.6(3) 4 . ? C13 O3 Li1 146.8(3) . . ? Li1 O3 Li1 84.5(3) 4 . ? Li2 O3 Li1 84.0(3) . . ? C13 O3 K2 93.1(2) . . ? Li1 O3 K2 72.7(2) 4 . ? Li2 O3 K2 144.9(2) . . ? Li1 O3 K2 72.4(2) . . ? C13 O3 K1 91.6(2) . . ? Li1 O3 K1 145.6(2) 4 . ? Li2 O3 K1 73.0(2) . . ? Li1 O3 K1 72.5(2) . . ? K2 O3 K1 121.37(10) . . ? C14 O4 Li2 119.8(3) . 4 ? C14 O4 Li1 120.2(3) . . ? Li2 O4 Li1 80.6(3) 4 . ? C14 O4 Li2 146.6(3) . . ? Li2 O4 Li2 83.6(3) 4 . ? Li1 O4 Li2 84.8(3) . . ? C14 O4 K1 92.7(2) . . ? Li2 O4 K1 145.6(2) 4 . ? Li1 O4 K1 72.8(2) . . ? Li2 O4 K1 72.9(2) . . ? C14 O4 K3 91.9(2) . . ? Li2 O4 K3 72.3(2) 4 . ? Li1 O4 K3 145.6(2) . . ? Li2 O4 K3 71.8(2) . . ? K1 O4 K3 121.01(9) . . ? C5 N1 C1 112.6(4) . . ? C5 N1 Li1 134.0(4) . . ? C1 N1 Li1 113.2(4) . . ? C5 N1 K1 91.2(3) . . ? C1 N1 K1 128.3(5) . . ? Li1 N1 K1 63.0(2) . . ? C5 N1 K2 87.9(3) . . ? C1 N1 K2 126.4(6) . . ? Li1 N1 K2 61.6(2) . . ? K1 N1 K2 98.30(11) . . ? C11 N2 C7 112.4(4) . . ? C11 N2 Li2 133.9(4) . . ? C7 N2 Li2 113.6(4) . . ? C11 N2 K3 92.7(3) . . ? C7 N2 K3 125.3(4) . . ? Li2 N2 K3 62.8(2) . . ? C11 N2 K1 86.4(3) . . ? C7 N2 K1 129.1(3) . . ? Li2 N2 K1 62.1(2) . . ? K3 N2 K1 98.77(10) . . ? C17 N3 C18 109.2(7) . . ? C17 N3 C15 111.3(7) . . ? C18 N3 C15 110.2(7) . . ? C17 N3 K1 119.0(5) . . ? C18 N3 K1 91.0(4) . . ? C15 N3 K1 114.1(4) . . ? C20 N4 C16 111.9(6) . . ? C20 N4 C19 110.2(5) . . ? C16 N4 C19 109.0(6) . . ? C20 N4 K1 94.5(4) . . ? C16 N4 K1 114.3(4) . . ? C19 N4 K1 116.2(4) . . ? C21 N5 C23 108.8(7) . . ? C21 N5 C22 107.6(6) . . ? C23 N5 C22 108.3(6) . . ? C21 N5 K2 109.1(3) . . ? C23 N5 K2 105.2(4) . . ? C22 N5 K2 117.6(4) . . ? C25 N6 C24 118.0(7) . . ? C25 N6 C26 105.3(8) . . ? C24 N6 C26 104.8(7) . . ? C25 N6 K3 110.0(5) . . ? C24 N6 K3 112.4(3) . . ? C26 N6 K3 104.9(5) . . ? C2 C1 N1 125.6(6) . . ? C2 C1 H1A 105.9 . . ? N1 C1 H1A 105.9 . . ? C2 C1 H1B 105.9 . . ? N1 C1 H1B 105.9 . . ? H1A C1 H1B 106.2 . . ? C1 C2 C3 123.8(6) . . ? C1 C2 H2A 106.4 . . ? C3 C2 H2A 106.4 . . ? C1 C2 H2B 106.4 . . ? C3 C2 H2B 106.4 . . ? H2A C2 H2B 106.4 . . ? C2 C3 C4 112.0(5) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 118.0(5) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N1 C5 O1 111.5(4) . . ? N1 C5 C4 127.0(5) . . ? O1 C5 C4 121.5(4) . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N2 115.0(6) . . ? C8 C7 H7A 108.5 . . ? N2 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? N2 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 C9 113.0(6) . . ? C7 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C8 109.8(5) . . ? C10 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 120.3(5) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 N2 128.8(5) . . ? C10 C11 O2 122.4(5) . . ? N2 C11 O2 108.8(4) . . ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 113.6(6) . . ? N3 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? N3 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? N4 C16 C15 112.7(6) . . ? N4 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? N4 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 C21 N5 125.7(4) 4 . ? C21 C21 H21A 105.9 4 . ? N5 C21 H21A 105.9 . . ? C21 C21 H21B 105.9 4 . ? N5 C21 H21B 105.9 . . ? H21A C21 H21B 106.2 . . ? N5 C22 H22A 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N5 C23 H23A 109.5 . . ? N5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C24 C24 121.0(5) . 4 ? N6 C24 H24A 107.1 . . ? C24 C24 H24A 107.1 4 . ? N6 C24 H24B 107.1 . . ? C24 C24 H24B 107.1 4 . ? H24A C24 H24B 106.8 . . ? N6 C25 H25A 109.5 . . ? N6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N6 C26 H26A 109.5 . . ? N6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O4 Li1 N1 120.4(4) . . ? O4 Li1 O3 100.0(3) . 4 ? N1 Li1 O3 122.3(4) . 4 ? O4 Li1 O3 94.9(3) . . ? N1 Li1 O3 118.5(3) . . ? O3 Li1 O3 94.7(3) 4 . ? O4 Li1 Li2 49.5(2) . 4 ? N1 Li1 Li2 144.7(4) . 4 ? O3 Li1 Li2 50.5(2) 4 4 ? O3 Li1 Li2 96.7(3) . 4 ? O4 Li1 Li1 93.6(2) . 4 ? N1 Li1 Li1 145.6(2) . 4 ? O3 Li1 Li1 48.2(2) 4 4 ? O3 Li1 Li1 47.4(2) . 4 ? Li2 Li1 Li1 61.6(2) 4 4 ? O4 Li2 N2 120.8(4) 4 . ? O4 Li2 O3 99.8(3) 4 . ? N2 Li2 O3 121.5(4) . . ? O4 Li2 O4 95.7(3) 4 . ? N2 Li2 O4 118.7(3) . . ? O3 Li2 O4 94.4(3) . . ? O4 Li2 Li1 49.9(2) 4 4 ? N2 Li2 Li1 144.2(4) . 4 ? O3 Li2 Li1 49.9(2) . 4 ? O4 Li2 Li1 97.1(3) . 4 ? O4 Li2 Li2 48.8(2) 4 4 ? N2 Li2 Li2 144.2(2) . 4 ? O3 Li2 Li2 94.0(2) . 4 ? O4 Li2 Li2 47.6(2) . 4 ? Li1 Li2 Li2 62.2(2) 4 4 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.695 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.065